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Sample records for sampling graphite furnace

  1. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  2. Solid sampling determination of magnesium in lithium niobate crystals by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Dravecz, Gabriella; Laczai, Nikoletta; Hajdara, Ivett; Bencs, László

    2016-12-01

    The vaporization/atomization processes of Mg in high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) were investigated by evaporating solid (powder) samples of lithium niobate (LiNbO3) optical single crystals doped with various amounts of Mg in a transversally heated graphite atomizer (THGA). Optimal analytical conditions were attained by using the Mg I 215.4353 nm secondary spectral line. An optimal pyrolysis temperature of 1500 °C was found for Mg, while the compromise atomization temperature in THGAs (2400 °C) was applied for analyte vaporization. The calibration was performed against solid (powered) lithium niobate crystal standards. The standards were prepared with exactly known Mg content via solid state fusion of the oxide components of the matrix and analyte. The correlation coefficient (R value) of the linear calibration was not worse than 0.9992. The calibration curves were linear in the dopant concentration range of interest (0.74-7.25 mg/g Mg), when dosing 3-10 mg of the powder samples into the graphite sample insertion boats. The Mg content of the studied 19 samples was in the range of 1.69-4.13 mg/g. The precision of the method was better than 6.3%. The accuracy of the results was verified by means of flame atomic absorption spectrometry with solution sample introduction after digestion of several crystal samples.

  3. [Detecting Thallium in Water Samples using Dispersive Liquid Phase Microextraction-Graphite Furnace Atomic Absorption Spectroscopy].

    Science.gov (United States)

    Zhu, Jing; Li, Yan; Zheng, Bo; Tang, Wei; Chen, Xiao; Zou, Xiao-li

    2015-11-01

    To develope a method of solvent demulsification dispersive liquid phase microextraction (SD-DLPME) based on ion association reaction coupled with graphite furnace atomic absorption spectroscopy (GFAAS) for detecting thallium in water samples. Methods Thallium ion in water samples was oxidized to Tl(III) with bromine water, which reacted with Cl- to form TlCl4-. The ionic associated compound with trioctylamine was obtained and extracted. DLPME was completed with ethanol as dispersive solvent. The separation of aqueous and organic phase was achieved by injecting into demulsification solvent without centrifugation. The extractant was collected and injected into GFAAS for analysis. With palladium colloid as matrix modifier, a two step drying and ashing temperature programming process was applied for high precision and sensitivity. The linear range was 0.05-2.0 microg/L, with a detection limit of 0.011 microg/L. The relative standard derivation (RSD) for detecting Tl in spiked water sample was 9.9%. The spiked recoveries of water samples ranged from 94.0% to 103.0%. The method is simple, sensitive and suitable for batch analysis of Tl in water samples.

  4. High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Santos, Rafael F.; Carvalho, Gabriel S.; Duarte, Fabio A.; Bolzan, Rodrigo C.; Flores, Erico M. M.

    2017-03-01

    In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10 mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 2.5, 1.7, 17 and 0.12 ng g- 1 for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration.

  5. Determination of platinum and palladium in environmental samples by graphite furnace atomic absorption spectrometry after separation on dithizone sorbent.

    Science.gov (United States)

    Chwastowska, J; Skwara, W; Sterlińska, E; Pszonicki, L

    2004-09-08

    A graphite furnace atomic absorption method of platinum and palladium determination after their separation from environmental samples has been presented. The samples were digested by aqua regia and the analyte elements were separated on the dithizone sorbent. The procedure of sorbent preparation was described and their properties were established. Two various procedures of elution by thiourea and concentrated nitric acid were described and discussed. The low limit of detection was established as 1ngg(-1) for platinum and 0.2ngg(-1) for palladium. There was also investigated the behaviour of platinum and palladium introduced into the soil in various chemical forms.

  6. Determination of vanadium in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry using permanent modifiers.

    Science.gov (United States)

    Dobrowolski, Ryszard; Adamczyk, Agnieszka; Otto, Magdalena

    2013-09-15

    A new analytical procedure for vanadium (V) determination in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry (slurry sampling GFAAS) using the mixed permanent modifiers is described. Moreover, the comparison of action of the modifiers based on the iridium (Ir) and carbide-forming elements: tungsten (W) and niobium (Nb) deposited on the graphite tubes is studied, especially in terms of their analytical utility and determination sensitivity. The mechanism of their action was investigated using an X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray detector (EDX). Finally, the mixture of 0.3 μg of Ir and 0.04 μg of Nb was used for the graphite tube permanent modification. The analytical procedure was optimized on the basis of the data from pyrolysis and atomization temperature curves studies. The results obtained for the four certified reference materials (marine sediments: PACS-1 and MESS-1, lake sediment: SL-1, soil: San Joaquin Soil SRM 2709), using the slurry sampling GFAAS and the standard calibration method, were in good agreement with the certified values. The detection and quantification limits and characteristic mass calculated for the proposed procedure were 0.04 µg/g, 0.16 µg/g and 11.9 pg, respectively. The precision (RSD% less than 8%) and the accuracy of vanadium determination in the soil and sediment samples were acceptable. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. [Determination of lead in water samples by graphite furnace atomic absorption spectrometry after cloud point extraction with dithizone].

    Science.gov (United States)

    Xiao, Shan-Mei; Chen, Jian-Rong; Shen, Yu-Qin

    2006-05-01

    Cloud point extraction was used for the preconcentration of lead after the formation of a complex with dithizone in the presence of surfactant Triton X-114, and then the lead was determined by graphite furnace atomic absorption spectrometry. The conditions affecting the separation and detection process were optimized. Separation of the two phases was accomplished by centrifugation for 15 min at 4 000 rpm. Upon cooling in an ice-bath, the surfactant-rich phase became viscous. The aqueous phase could then be separated by inverting the tubes. Later, a solution of methanol containing 0.1 mol x L(-1) of HNO3 was added to the surfactant-rich phase up to 0.5 mL. The samples were determined by graphite furnace atomic absorption spectrometry with NH4H2PO4 and Mg(NO3)2 as a chemical modifier. At pH 8.0, the preconcentration of only 10 mL sample in the presence of 0.05% Triton X-114 and 20 micromol x L(-1) dithizone permitted the detection of 0.089 microg x L(-1) lead. The enhancement factors were 19.1 times for lead. The calibration graph using the preconcentration system for lead was linear with a correlation coefficient of 0.998 from levels near the detection limits up to at least 30 microg x L(-1). The regression equation was A = 0.026 1c (microg x L(-1)) + 0.010 6. The proposed method has been applied to the determination of lead in water samples.

  8. Selective cloud point extraction and graphite furnace atomic absorption spectrometric determination of molybdenum (VI) ion in seawater samples

    Energy Technology Data Exchange (ETDEWEB)

    Filik, Hayati, E-mail: filik@istanbul.edu.tr [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey); Cengel, Tayfun; Apak, Resat [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey)

    2009-09-30

    A cloud point extraction process using the nonionic surfactant Triton X-114 to extract molybdenum from aqueous solutions was investigated. The method is based on the complexation reaction of Mo(VI) with 1,2,5,8-tetrahydroxyanthracene-9,10-dione (quinalizarine: QA) and micelle-mediated extraction of the complex. The enriched analyte in the surfactant-rich phase was determined by graphite furnace atomic absorption spectrometry (GFAAS). The optimal extraction and reaction conditions (e.g. pH, reagent and surfactant concentrations, temperature, incubation and centrifugation times) were evaluated and optimized. Under the optimized experimental conditions, the limit of detection (LOD) for Mo(VI) was 7.0 ng L{sup -1} with an preconcentration factor of {approx}25 when 10 mL of sample solution was preconcentrated to 0.4 mL. The proposed method (with extraction) showed linear calibration within the range 0.03-0.6 {mu}g L{sup -1}. The relative standard deviation (RSD) was found to be 3.7% (C{sub Mo(VI)} = 0.05 {mu}g L{sup -1}, n = 5) for pure standard solutions, whereas RSD for the recoveries from real samples ranged between 2 and 8% (mean RSD = 3.9%). The method was applied to the determination of Mo(VI) in seawater and tap water samples with a recovery for the spiked samples in the range of 98-103%. The interference effect of some cations and anions was also studied. In the presence of foreign ions, no significant interference was observed. In order to verify the accuracy of the method, a certified reference water sample was analysed and the results obtained were in good agreement with the certified values.

  9. Solid sampling determination of total fluorine in baby food samples by high-resolution continuum source graphite furnace molecular absorption spectrometry.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-11-15

    This study describes the applicability of solid sampling technique for the determination of fluorine in various baby foods via molecular absorption of calcium monofluoride generated in a graphite furnace of high-resolution continuum source atomic absorption spectrometry. Fluorine was determined at CaF wavelength, 606.440nm in a graphite tube applying a pyrolysis temperature of 1000°C and a molecule forming temperature of 2200°C. The limit of detection and characteristic mass of the method were 0.20ng and 0.17ng of fluorine, respectively. The fluorine concentrations determined in standard reference sample (bush branches and leaves) were in good agreement with the certified values. By applying the optimized parameters, the concentration of fluorine in various baby foods were determined. The fluorine concentrations were ranged from sample amounts used in solid sampling analysis, micro-scale distribution of fluorine in the samples was also determined. Copyright © 2016 Elsevier Ltd. All rights reserved.

  10. Comparison of different sample preparation methods for platinum determination in cultured cells by graphite furnace atomic absorption spectrometry

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    Man Xiao

    2017-01-01

    Full Text Available Background Platinum-based agents are widely used in chemotherapy against solid tumors and insufficient intracellular drug accumulation is one of the leading causes of platinum resistance which is associated with poor survival of tumor patients. Thus, the detection of intracellular platinum is pivotal for studies aiming to overcome platinum resistance. In the present study, we aimed to establish a reliable graphite furnace atomic absorption spectrometry (GFAAS-based assay to quantify the intracellular platinum content for cultured cells. Methods Several most commonly applied cell preparation methods, including 0.2% HNO3, 0.2% Triton X-100, concentrated nitric acid, RIPA combined with concentrated nitric acid and hydroxide, followed by GFAAS for platinum detection were compared in ovarian, cervical and liver cancer cell lines to obtain the optimal one, and parameters regarding linearity, accuracy, precision and sensitivity were evaluated. Influence of other metals on platinum detection and the storage conditions of samples were also determined. Results The treatment of cells with 0.2% HNO3 was superior to other approaches with fewer platinum loss and better repeatability. The recovery rate and precision of this method were 97.3%–103.0% and 1.4%–3.8%, respectively. The average recoveries in the presence of other metals were 95.1%–103.1%. The detection limit was 13.23 ug/L. The recovery rate of platinum remained acceptable even in cell samples stored in −20 °C or −80 °C for two months. Discussion After comparison, we found that 0.2% HNO3 was optimal for intracellular platinum quantification based on GFAAS, which presented values compatible with that of inductively-coupled plasma mass-spectrometry (ICP-MS, and this is partially attributed to the simplicity of this method. Moreover, the assay was proved to be accurate, sensitive, cost-effective and suitable for the research of platinum-based antitumor therapy.

  11. Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for gold determination in geological samples after preconcentration onto carbon nanotubes

    Science.gov (United States)

    Dobrowolski, Ryszard; Mróz, Agnieszka; Dąbrowska, Marzena; Olszański, Piotr

    2017-06-01

    A novelty method for the determination of gold in geological samples by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GF AAS) after solid-phase extraction onto modified carbon nanotubes (CNT) was described. The methodology developed is based on solid phase extraction of Au(III) ions from digested samples to eliminate strong interference caused by iron compounds and problems related to inhomogeneities of the samples. The use of aqueous or solid standard for calibration was studied and the slope of calibration curve was the same for both of these modes. This statement indicates the possibility to perform the calibration of the method using aqueous standard solutions. Under optimum conditions the absolute detection limit for gold was equal to 2.24 · 10- 6 μg g- 1 while the adsorption capacity of modified carbon nanotubes was 264 mg g- 1. The proposed procedure was validated by the application of certified reference materials (CRMs) with different content of gold and different matrix, the results were in good agreement with certified values. The method was successfully applied for separation and determination of gold ions in complex geological samples, with precision generally better than 8%.

  12. Solid sampling graphite furnace atomic absorption spectrometry for the direct analysis of microextraction solvent bars used for metal ultra-trace pre-concentration

    Science.gov (United States)

    González-Álvarez, Rafael Jesús; Pinto, Juan J.; Bellido-Milla, Dolores; Moreno, Carlos

    2017-09-01

    The potential applicability of the continuum source solid sampling graphite furnace atomic absorption spectroscopy (CS SS-GF AAS) technique has been studied to carry out the direct analysis of microextraction solvent bars used for metal ultra-trace pre-concentration in natural waters. An optimisation of the temperature program was developed for this purpose. Preliminary chamber furnace studies were performed in order to understand the behaviour of the bars with the increasing temperature. Solvent bars were filled with an acceptor solution, impregnated with an organic extractant and placed into the chamber furnace to carry out several temperature programs. Results led to perform a correct optimisation of the drying and pyrolysis steps of the furnace temperature program, which was tested with silver once completed. Blank solvent bars as well as standards containing silver were measured, obtaining a calibration curve with a correlation coefficient of 0.991. The results exhibited good repeatability and reproducibility, with relative standard deviations below 10% in both cases, indicating a promising applicability of the CS SS-GF AAS technique to directly determine metallic species in microextraction solvent bars.

  13. Investigation of spectral interferences in the determination of lead in fertilizers and limestone samples using high-resolution continuum source graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Becker, Emilene M.; François, Luciane L.; Jesus, Alexandre de [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2014-11-01

    In the present work, spectral interferences on the determination of lead in fertilizer and limestone samples were investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry at the main analytical lines: 217.001 and 283.306 nm. For these investigations, samples were introduced into the furnace as slurry together with a mixture of Pd and Mg as chemical modifier. Spectral interferences were observed for some samples at both analytical lines. In order to verify whether a wet digestion procedure would avoid these interferences, a reference method for wet digestion of fertilizers was employed as an alternative sample preparation procedure. However, the same interferences were also observed in the digested samples. In order to identify and eliminate the fine-structured background using a least-squares background correction, reference spectra were generated using the combination of different species. The use of the latter technique allowed the elimination of spectral interferences for most of the investigated samples, making possible the determination of lead in fertilizer and limestone samples free of interferences. The best results were found using a reference spectrum of NH{sub 4}H{sub 2}PO{sub 4} at 217.001 nm, and a mixture of H{sub 2}SO{sub 4} + Ca and HNO{sub 3} + Ca at the 283.306 nm line. The accuracy of the method was evaluated using a certified reference material “Trace Elements in Multi-Nutrient Fertilizer”. Similar results were obtained using line source graphite furnace atomic absorption spectrometry with Zeeman-effect background correction, indicating that the latter technique was also capable to correct the spectral interferences, at least in part. - Highlights: • Spectral interferences on the determination of lead in fertilizers and limestone. • The analytical lines at 217.001 nm and 283.306 nm using HR-CS GF AAS. • Various combinations of compounds were used to create reference spectra. • LSBC

  14. Direct determination of Pb in raw milk by graphite furnace atomic absorption spectrometry (GF AAS) with electrothermal atomization sampling from slurries.

    Science.gov (United States)

    de Oliveira, Tatiane Milão; Augusto Peres, Jayme; Lurdes Felsner, Maria; Cristiane Justi, Karin

    2017-08-15

    Milk is an important food in the human diet due to its physico-chemical composition; therefore, it is necessary to monitor contamination by toxic metals such as Pb. Milk sample slurries were prepared using Triton X-100 and nitric acid for direct analysis of Pb using graphite furnace atomic absorption spectrometry - GF AAS. After dilution of the slurries, 10.00µl were directly introduced into the pyrolytic graphite tube without use of a chemical modifier, which acts as an advantage considering this type of matrix. The limits of detection and quantification were 0.64 and 2.14µgl(-1), respectively. The figures of merit studied showed that the proposed methodology without pretreatment of the raw milk sample and using external standard calibration is suitable. The methodology was applied in milk samples from the Guarapuava region, in Paraná State (Brazil) and Pb concentrations ranged from 2.12 to 37.36µgl(-1). Copyright © 2017 Elsevier Ltd. All rights reserved.

  15. High-resolution continuum source graphite furnace molecular absorption spectrometry compared with ion chromatography for quantitative determination of dissolved fluoride in river water samples.

    Science.gov (United States)

    Ley, Philip; Sturm, Manfred; Ternes, Thomas A; Meermann, Björn

    2017-10-03

    In addition to beneficial health effects, fluoride can also have adverse effects on humans, animals, and plants if the daily intake is strongly elevated. One main source of fluoride uptake is water, and thus several ordinances exist in Germany that declare permissible concentrations of fluoride in, for example, drinking water, mineral water, and landfill seepage water. Controlling the fluoride concentrations in aqueous matrices necessitate valid and fast analytical methods. In this work an alternative method for the determination of fluoride in surface waters based on high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) was applied. Fluoride detection was made possible by the formation of a diatomic molecule, GaF, and detection of characteristic molecular absorption. On HR-CS-GFMAS parameter optimization, the method was adapted to surface water sample analysis. The influence of potential main matrix constituents such as Na+, Ca2+, Mg2+, and Cl- as well as surface water sampling/storage conditions on the molecular absorption signal of GaF was investigated. Method validation demonstrated a low limit of detection (8.1 μg L-1) and a low limit of quantification (26.9 μg L-1), both sufficient for direct river water sample analysis after 0.45-μm filtration. The optimized HR-CS-GFMAS method was applied for the analysis of real water samples from the rivers Rhine and Moselle. For method validation, samples were also analyzed by an ion chromatography (IC) method. IC and HR-CS-GFMAS results both agreed well. In comparison with IC, HR-CS-GFMAS has higher sample throughput, a lower limit of detection and a lower limit of quantification, and higher selectivity, and is a very suitable method for the analysis of dissolved fluoride in river water. Graphical abstract High-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) was applied for the quantitative analysis of dissolved fluoride in river

  16. Micro-sampling method based on high-resolution continuum source graphite furnace atomic absorption spectrometry for calcium determination in blood and mitochondrial suspensions.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Mª Jesús; Sevilla, Mª Teresa; Satrústegui, Jorgina; Procopio, Jesús R

    2017-08-01

    A micro-sampling and straightforward method based on high resolution continuum source atomic absorption spectrometry (HR-CS AAS) was developed to determine extracellular and intracellular Ca in samples of interest in clinical and biomedical analysis. Solid sampling platforms were used to introduce the micro-samples into the graphite furnace atomizer. The secondary absorption line for Ca, located at 239.856nm, was selected to carry out the measurements. Experimental parameters such as pyrolysis and atomization temperatures and the amount of sample introduced for the measurements were optimized. Calibration was performed using aqueous standards and the approach to measure at the wings of the absorption lines was employed for the expansion of the linear response range. The limit of detection was of 0.02mgL-1 Ca (0.39ng Ca) and the upper limit of linear range was increased up to 8.0mgL-1 Ca (160ng Ca). The proposed method was used to determine Ca in mitochondrial suspensions and whole blood samples with successful results. Adequate recoveries (within 91-107%) were obtained in the tests performed for validation purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Determination of Al, Cu, Li and Mn in spruce seeds and plant reference materials by slurry sampling graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Engelsen, C; Wibetoe, G

    2000-03-01

    An ultrasonic slurry sampling graphite furnace AAS method was developed for the determination of Al, Cu, Li and Mn in spruce seeds, NBS SRM 1575 pine needles and GBW CRM 07602 bush branches and leaves. The only sample preparation was grinding in a Mixer Mill before preparing a slurry by adding 0.14 mol/L nitric acid to a small sample aliquot. Cryogenic grinding was used for the spruce seeds to solve the problem of agglomerating during grinding at room temperature. A modified sample tray was applied allowing the use of both the commercial 1.5 mL vials and home-made 15 mL vials. With optimal conditions for ultrasonic agitation the homogeneity and particle size distributions in the slurries prepared in the two different vials were similar. Several aspects of the slurry sampling approach are discussed and data of important parameters are given, including the total number of particles injected into the graphite furnace, densities of the materials and percentage of analyte extracted into the liquid phase of the slurry. The density of the materials was determined by two methods; by using a Coulter particle analyser and by using a gravimetric method. The two methods gave similar accuracy and precision. The concentration ranges of the elements (in microg g(-1)) were: 80-2100 for Al, 3-15 for Cu, 0.06-2.5 for Li and 50-700 for Mn. External calibration with aqueous standards was employed. Chemical modifiers were not found to be necessary. The relative standard deviations were in the range 1.7-7%. Analyses of the two certified plant reference materials confirmed the accuracy of the method. In addition no significant difference was found for analyses of digested and slurried spruce seeds. The detection limit was 10 ng g(-1) for Li and 170 ng g(-1) for Cu. The characteristic mass (area measurements) was 4.4 pg for Li and 11 pg for Cu. For Al and Mn less sensitive wavelengths were used.

  18. Investigation of chemical modifiers for sulfur determination in diesel fuel samples by high-resolution continuum source graphite furnace molecular absorption spectrometry using direct analysis

    Energy Technology Data Exchange (ETDEWEB)

    Huber, Charles S. [Instituto Federal Sul-rio-grandense, Câmpus Pelotas, Pelotas, RS (Brazil); Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Universidade Federal de Santa Catarina, Departamento de Química, Florianópolis, SC (Brazil); Andrade, Jailson B. [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2015-06-01

    High-resolution continuum source graphite furnace molecular absorption spectrometry has been applied for sulfur determination in diesel fuel. The sharp rotational lines of the carbon monosulfide molecule (formed during the vaporization step) were used to measure the absorbance. The analytical line at 258.056 nm was monitored using the sum of three pixels. Different chemical modifiers were investigated and the mixture of palladium and magnesium was used as chemical modifier in combination with iridium as permanent modifier. L-Cysteine was chosen as sulfur standard and the calibration was done against aqueous standard solutions. The proposed method was applied for the analyses of four diesel samples: two S10 samples and two S500 samples. The trueness of the method was checked with a certified reference material (CRM) of sulfur in diesel fuel (NIST 2724b). Accurate results, for samples and CRM, were achieved after a dilution with propan-1-ol. The following figures of merit were obtained: characteristic mass of 17 ± 3 ng, limit of detection and limit of quantification of 1.4 mg kg{sup −1} and 4.7 mg kg{sup −1}, respectively. - Highlights: • Ir, Ru and Zr were investigated as permanent modifiers. • Ca, Mg, Pd and Pd/Mg were investigated as modifiers in solution. • Indirect determination of sulfur monitoring the molecular absorbance of the CS • Direct analysis of diesel samples using a dilution in propan-1-ol.

  19. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    Energy Technology Data Exchange (ETDEWEB)

    Virgilio, Alex; Nobrega, Joaquim A. [Department of Chemistry, Federal University of Sao Carlos, Post Office Box 676, 13560-970, Sao Carlos-SP (Brazil); Rego, Jardes F. [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil); Neto, Jose A. Gomes, E-mail: anchieta@iq.unesp.br [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil)

    2012-12-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 Degree-Sign C and 2400 Degree-Sign C, respectively. Slopes of calibration curves (50-750 pg Cr, R{sup 2} > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 {mu}g g{sup -1} Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 {+-} 2.1 {mu}g g{sup -1} Cr. The limit of detection was 3.3 ng g{sup -1} Cr. - Highlights: Black-Right-Pointing-Pointer Direct solid sampling is first time employed for Cr in plant materials. Black-Right-Pointing-Pointer Calibration curves with liquids and solids are coincident. Black-Right-Pointing-Pointer Microanalysis of plants for Cr is validated by reference materials. Black-Right-Pointing-Pointer The proposed HR-CS GF AAS method is environmental friendly.

  20. Magnetic stirrer induced dispersive ionic-liquid microextraction for the determination of vanadium in water and food samples prior to graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa

    2015-04-01

    A new dispersive liquid-liquid microextraction, magnetic stirrer induced dispersive ionic-liquid microextraction (MS-IL-DLLME) was developed to quantify the trace level of vanadium in real water and food samples by graphite furnace atomic absorption spectrometry (GFAAS). In this extraction method magnetic stirrer was applied to obtained a dispersive medium of 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6] in aqueous solution of (real water samples and digested food samples) to increase phase transfer ratio, which significantly enhance the recovery of vanadium - 4-(2-pyridylazo) resorcinol (PAR) chelate. Variables having vital role on desired microextraction methods were optimised to obtain the maximum recovery of study analyte. Under the optimised experimental variables, enhancement factor (EF) and limit of detection (LOD) were achieved to be 125 and 18 ng L(-1), respectively. Validity and accuracy of the desired method was checked by analysis of certified reference materials (SLRS-4 Riverine water and NIST SRM 1515 Apple leaves). The relative standard deviation (RSD) for 10 replicate determinations at 0.5 μg L(-1) of vanadium level was found to be <5.0%. This method was successfully applied to real water and acid digested food samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

  1. Graphite furnace atomic absorption spectrometric detection of vanadium in water and food samples after solid phase extraction on multiwalled carbon nanotubes.

    Science.gov (United States)

    Wadhwa, Sham Kumar; Tuzen, Mustafa; Gul Kazi, Tasneem; Soylak, Mustafa

    2013-11-15

    Vanadium(V) ions as 8-hydroxyquinoline chelates were loaded on multiwalled carbon nanotubes (MWNTs) in a mini chromatographic column. Vanadium was determined by graphite furnace atomic absorption spectrometry (GFAAS). Various analytical parameters including pH of the working solutions, amounts of 8-hydroxyquinoline, eluent type, sample volume, and flow rates were investigated. The effects of matrix ions and some transition metals were also studied. The column can be reused 250 times without any loss in its sorption properties. The preconcentration factor was found as 100. Detection limit (3 s) and limit of quantification (10 s) for the vanadium in the optimal conditions were observed to be 0.012 µg L(-1) and 0.040 μg L(-1), respectively. The capacity of adsorption was 9.6 mg g(-1). Relative standard deviation (RSD) was found to be 5%. The validation of the method was confirmed by using NIST SRM 1515 Apple leaves, NIST SRM 1570a Spinach leaves and GBW 07605 Tea certified reference materials. The procedure was applied to the determination of vanadium in tap water and bottled drinking water samples. The procedure was also successfully applied to microwave digested food samples including black tea, coffee, tomato, cabbage, zucchini, apple and chicken samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. One-step displacement dispersive liquid-liquid microextraction coupled with graphite furnace atomic absorption spectrometry for the selective determination of methylmercury in environmental samples.

    Science.gov (United States)

    Liang, Pei; Kang, Caiyan; Mo, Yajun

    2016-01-01

    A novel method for the selective determination of methylmercury (MeHg) was developed by one-step displacement dispersive liquid-liquid microextraction (D-DLLME) coupled with graphite furnace atomic absorption spectrometry. In the proposed method, Cu(II) reacted with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which was used as the chelating agent instead of DDTC for the dispersive liquid-liquid microextraction (DLLME) of MeHg. Because the stability of MeHg-DDTC is higher than that of Cu-DDTC, MeHg can displace Cu from the Cu-DDTC complex and be preconcentrated in a single DLLME procedure. MeHg could be extracted into the extraction solvent phase at pH 6 while Hg(II) remained in the sample solution. Potential interference from co-existing metal ions with lower DDTC complex stability was largely eliminated without the need of any masking reagent. Under the optimal conditions, the limit of detection of this method was 13.6ngL(-1) (as Hg), and an enhancement factor of 81 was achieved with a sample volume of 5.0mL. The proposed method was successfully applied for the determination of trace MeHg in some environmental samples with satisfactory results. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Determination of macro and trace elements in multivitamin dietary supplements by high-resolution continuum source graphite furnace atomic absorption spectrometry with slurry sampling.

    Science.gov (United States)

    Krawczyk, Magdalena

    2014-01-01

    In this research, three different commercially available multivitamin dietary supplements were analyzed by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) with slurry sampling. The concentrations of Cr, Cu, Fe, Mn, and Se were determined and compared to the amounts stated by producers. The safety of multivitamin dietary supplements depends on various factors including the manufacturing process and the purity and origins of the raw ingredients. For this reason, this research determined concentrations of several toxic elements (As, Cd, and Pb). Microwave-assisted high pressure Teflon bomb digestion was used to determine total amounts of elements in samples. Samples were prepared as slurries at a concentration of 0.1% (m/v) for macro elements (Cr, Cu, Fe, Mn, and Se) and at a concentration of % (m/v) for trace elements (As, Cd, and Pb) in acidic media (3M HNO3). The influence of acid concentration, Triton X-100 addition, sonication time, and sonication power on absorbance was investigated. The accuracy of this method was validated by analyses of NRCC LUTS-1 (Lobster hepatopancreas), NRCC DORM-1 (Dogfish Muscle), NRCC DOLT-2 (Dogfish Liver), NBS SRM 1570 (Spinach Leaves) and NBS SRM 1573 (Tomato Leaves) certified reference materials. The measured elements contents in these reference materials (except NRCC DOLT-2) were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Evaluation of solid sampling for determination of Mo, Ni, Co, and V in soil by high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Babos, Diego Victor; Barros, Ariane Isis; Ferreira, Edilene Cristina; Neto, José Anchieta Gomes

    2017-04-01

    New methods are proposed for the determination of Mo, Ni, Co, and V in soils using high-resolution continuum source graphite furnace atomic absorption spectrometry with direct solid sampling. Cobalt and V were simultaneously determined, and different analytical lines of Ni and V were monitored to adjust sensitivity for each sample. Accuracy was checked by means of soil certified reference materials, and also by flame atomic absorption spectrometry as comparative technique. The results for Mo, Ni, Co, and V found by proposed methods were in agreement with certified values and with those obtained by the comparative technique at 95% confidence level. The concentrations found in different soil samples were in the ranges 0.19-1.84 mg kg- 1 (Mo), 9.2-22.7 mg kg- 1 (Ni), 1.1-10.7 mg kg- 1 (Co), and 35.6-426.1 mg kg- 1 (V). The relative standard deviations were in the ranges 3.2-10% (Mo), 2.8-9.8% (Ni), 4.0-9.2% (Co), and 1.2-8.0% (V). The limits of quantification for Mo, Ni, Co, and V were 0.027, 0.071, 0.15, and 1.43 ng, respectively.

  5. Determination of Lead in Water Samples Using a New Vortex-Assisted, Surfactant-Enhanced Emulsification Liquid-Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry.

    Science.gov (United States)

    Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Pan, Weiliang; Tang, Xiaohui; Zhou, Guangming; Mao, Yufeng; Su, Xaioxuan

    2016-04-01

    A low toxic solvent-based vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction (LT-VSLLME) combined with graphite furnace atomic absorption spectrometry was developed for the extraction and determination of lead (Pb) in water samples. In the LT-VSLLME method, the extraction solvent was dispersed into the aqueous samples by the assistance of vortex agitator. Meanwhile, the addition of a surfactant, which acted as an emulsifier, could enhance the speed of the mass-transfer from aqueous samples to the extraction solvent. The influences of analytical parameters, including extraction solvent type and its volume, surfactant type and its volume, pH, concentration of chelating agent, salt effect and extraction time were investigated. Under the optimized conditions, a good relative standard deviation of 3.69% at 10 ng L(-1) was obtained. The calibration graph showed a linear pattern in the ranges of 5-30 ngL(-1), with a limit of detection of 0.76 ng L(-1). The linearity was obtained by five points in the concentration range of 5-30 ngL(-1). The enrichment factor was 320. The procedure was applied to wastewater and river water, and the accuracy was assessed through the analysis of the recovery experiments.

  6. Simultaneous determination of V, Ni and Fe in fuel fly ash using solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Cárdenas Valdivia, A; Vereda Alonso, E; López Guerrero, M M; Gonzalez-Rodriguez, J; Cano Pavón, J M; García de Torres, A

    2018-03-01

    A green and simple method has been proposed in this work for the simultaneous determination of V, Ni and Fe in fuel ash samples by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GFAAS). The application of fast programs in combination with direct solid sampling allows eliminating pretreatment steps, involving minimal manipulation of sample. Iridium treated platforms were applied throughout the present study, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9931. The concentrations found in the fuel ash samples analysed ranged from 0.66% to 4.2% for V, 0.23-0.7% for Ni and 0.10-0.60% for Fe. Precision (%RSD) were 5.2%, 10.0% and 9.8% for V, Ni and Fe, respectively, obtained as the average of the %RSD of six replicates of each fuel ash sample. The optimum conditions established were applied to the determination of the target analytes in fuel ash samples. In order to test the accuracy and applicability of the proposed method in the analysis of samples, five ash samples from the combustion of fuel in power stations, were analysed. The method accuracy was evaluated by comparing the results obtained using the proposed method with the results obtained by ICP OES previous acid digestion. The results showed good agreement between them. The goal of this work has been to develop a fast and simple methodology that permits the use of aqueous standards for straightforward calibration and the simultaneous determination of V, Ni and Fe in fuel ash samples by direct SS HR CS GFAAS. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Method development for the determination of bromine in coal using high-resolution continuum source graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Science.gov (United States)

    Pereira, Éderson R.; Castilho, Ivan N. B.; Welz, Bernhard; Gois, Jefferson S.; Borges, Daniel L. G.; Carasek, Eduardo; de Andrade, Jailson B.

    2014-06-01

    This work reports a simple approach for Br determination in coal using direct solid sample analysis in a graphite tube furnace and high-resolution continuum source molecular absorption spectrometry. The molecular absorbance of the calcium mono-bromide (CaBr) molecule has been measured using the rotational line at 625.315 nm. Different chemical modifiers (zirconium, ruthenium, palladium and a mixture of palladium and magnesium nitrates) have been evaluated in order to increase the sensitivity of the CaBr absorption, and Zr showed the best overall performance. The pyrolysis and vaporization temperatures were 800 °C and 2200 °C, respectively. Accuracy and precision of the method have been evaluated using certified coal reference materials (BCR 181, BCR 182, NIST 1630a, and NIST 1632b) with good agreement (between 98 and 103%) with the informed values for Br. The detection limit was around 4 ng Br, which corresponds to about 1.5 μg g- 1 Br in coal, based on a sample mass of 3 mg. In addition, the results were in agreement with those obtained using electrothermal vaporization inductively coupled plasma mass spectrometry, based on a Student t-test at a 95% confidence level. A mechanism for the formation of the CaBr molecule is proposed, which might be considered for other diatomic molecules as well.

  8. On-line preconcentration of ultra-trace thallium(I in water samples with titanium dioxide nanoparticles and determination by graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Saeid Asadpour

    2016-11-01

    Full Text Available A new method has been developed for the determination of Tl(I based on simultaneous sorption and preconcentration with a microcolumn packed with TiO2 nanoparticle with a high specific surface area prepared by Sonochemical synthesis prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS. The optimum experimental parameters for preconcentration of thallium, such as elution condition, pH, and sample volume and flow rate have been investigated. Tl(I can be quantitatively retained by TiO2 nanoparticles at pH 9.0, then eluted completely with 1.0 mol L−1 HCl. The adsorption capacity of TiO2 nanoparticles for Tl(I was found to be 25 mg g−1. Also detection limit, precision (RSD, n = 8 and enrichment factor for Tl(I were 87 ng L−1, 6.4% and 100, respectively. The method has been applied for the determination of trace amounts of Tl(I in some environmental water samples with satisfactory results.

  9. Direct solid sample analysis with graphite furnace atomic absorption spectrometry—a fast and reliable screening procedure for the determination of inorganic arsenic in fish and seafood.

    Science.gov (United States)

    Zmozinski, Ariane V; Llorente-Mirandes, Toni; Damin, Isabel C F; López-Sánchez, José F; Vale, Maria Goreti R; Welz, Bernhard; Silva, Márcia M

    2015-03-01

    Direct solid sample analysis with graphite furnace atomic absorption spectrometry (SS-GF AAS) was investigated initially with the intention of developing a method for the determination of total As in fish and other seafood. A mixture of 0.1% Pd+0.06% Mg+0.06% Triton X-100 was used as the chemical modifier, added in solution over the solid samples, making possible the use of pyrolysis and atomization temperatures of 1200 °C and 2400 °C, respectively. The sample mass had to be limited to 0.25 mg, as the integrated absorbance did not increase further with increasing sample mass. Nevertheless, the recovery of As from several certified reference materials was of the order of 50% lower than the certified value. Strong molecular absorption due to the phosphorus monoxide molecule (PO) was observed with high-resolution continuum source AAS (HR CS AAS), which, however, did not cause any spectral interference. A microwave-assisted digestion with HNO3/H2O2 was also investigated to solve the problem; however, the results obtained for several certified reference materials were statistically not different from those found with direct SS-GF AAS. Accurate values were obtained using inductively coupled plasma mass spectrometry (ICP-MS) to analyze the digested samples, which suggested that organic As compounds are responsible for the low recoveries. HPLC-ICP-MS was used to determine the arsenobetaine (AB) concentration. Accurate results that were not different from the certified values were obtained when the AB concentration was added to the As concentration found by SS-GF AAS for most certified reference materials (CRM) and samples, suggesting that SS-GF AAS could be used as a fast screening procedure for inorganic As determination in fish and seafood. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Direct determination of bromine in plastic materials by means of solid sampling high-resolution continuum source graphite furnace molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Flórez, M.R.; Resano, M., E-mail: mresano@unizar.es

    2013-10-01

    This work investigates the potential of high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of bromine in polymers, which could be interesting in view of the current regulations restricting the use of organobrominated compounds. The method developed is based on the addition of Ca (300 μg) and Pd (30 μg) to favor the formation of CaBr, which is monitored at the main molecular “lines” (rotational spectra) found in the vicinity of 625.315 nm. It was found that accurate results could be obtained for all the samples investigated (polyethylene, polypropylene and acrylonitrile butadiene styrene certified reference materials) using any of the lines studied and constructing the calibration curve with aqueous standards. Furthermore, the combined use of the main four CaBr lines available in the spectral area simultaneously monitored permits to easily expand the linear range up to 2000 ng, provides a limit of detection of 1.8 ng (1.8 μg g{sup −1} for a mass of 1 mg) and further improves precision to values between 3–7% RSD. Overall, the method proposed seems suited for the fast and simple control of these types of samples (approximately 10 min for sample are required), circumventing the traditional problems associated with sample digestion (e.g., losses of volatile compounds), and providing sufficient sensitivity to easily comply with regulations. - Highlights: • Owing to the extended use of BFRs, Br determination in plastics is of great interest. • Solid sampling HR CS GFMAS permits the direct determination of Br, as CaBr, in plastics. • A fast and simple methodology with aqueous standards for calibration is proposed. • A LOD of 1.8 μg g{sup −1} and precision values in the 3–7% RSD range are achieved.

  11. Multiple response optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry with sample injection as detergent emulsion

    Science.gov (United States)

    Brum, Daniel M.; Lima, Claudio F.; Robaina, Nicolle F.; Fonseca, Teresa Cristina O.; Cassella, Ricardo J.

    2011-05-01

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO 3, the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO 3 medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  12. Multiple response optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry with sample injection as detergent emulsion

    Energy Technology Data Exchange (ETDEWEB)

    Brum, Daniel M.; Lima, Claudio F. [Departamento de Quimica, Universidade Federal de Vicosa, A. Peter Henry Rolfs s/n, Vicosa/MG, 36570-000 (Brazil); Robaina, Nicolle F. [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil); Fonseca, Teresa Cristina O. [Petrobras, Cenpes/PDEDS/QM, Av. Horacio Macedo 950, Ilha do Fundao, Rio de Janeiro/RJ, 21941-915 (Brazil); Cassella, Ricardo J., E-mail: cassella@vm.uff.br [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil)

    2011-05-15

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO{sub 3}, the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO{sub 3} medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  13. Determination of mercury in airborne particulate matter collected on glass fiber filters using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling

    Energy Technology Data Exchange (ETDEWEB)

    Araujo, Rennan G.O., E-mail: rgoa01@terra.com.br [Laboratorio de Quimica Analitica Ambiental, Departamento de Quimica, Universidade Federal de Sergipe, Campus Sao Cristovao, 49.100-000, Sao Cristovao, SE (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Vignola, Fabiola; Castilho, Ivan N.B. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Borges, Daniel L.G.; Welz, Bernhard [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Vale, Maria Goreti R. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal do Rio Grande do Sul, 91501-970 Porto Alegre, RS (Brazil); Smichowski, Patricia [Comision Nacional de Energia Atomica (CNEA) and Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET), Buenos Aires (Argentina); Ferreira, Sergio L.C. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal da Bahia, 40170-290, Salvador, BA (Brazil); Becker-Ross, Helmut [Leibniz-Institut fuer Analytische Wissenschaften-ISAS-e.V., Department Berlin, 12489 Berlin (Germany)

    2011-05-15

    A study has been undertaken to assess the capability of high-resolution continuum source graphite furnace atomic absorption spectrometry for the determination of mercury in airborne particulate matter (APM) collected on glass fiber filters using direct solid sampling. The main Hg absorption line at 253.652 nm was used for all determinations. The certified reference material NIST SRM 1648 (Urban Particulate Matter) was used to check the accuracy of the method, and good agreement was obtained between published and determined values. The characteristic mass was 22 pg Hg. The limit of detection (3{sigma}), based on ten atomizations of an unexposed filter, was 40 ng g{sup -1}, corresponding to 0.12 ng m{sup -3} in the air for a typical air volume of 1440 m{sup 3} collected within 24 h. The limit of quantification was 150 ng g{sup -1}, equivalent to 0.41 ng m{sup -3} in the air. The repeatability of measurements was better than 17% RSD (n = 5). Mercury concentrations found in filter samples loaded with APM collected in Buenos Aires, Argentina, were between < 40 ng g{sup -1} and 381 {+-} 24 ng g{sup -1}. These values correspond to a mercury concentration in the air between < 0.12 ng m{sup -3} and 1.47 {+-} 0.09 ng m{sup -3}. The proposed procedure was found to be simple, fast and reliable, and suitable as a screening procedure for the determination of mercury in APM samples.

  14. Direct sample introduction of wines in graphite furnace atomic absorption spectrometry for the simultaneous determination of arsenic, cadmium, copper and lead content.

    Science.gov (United States)

    Ajtony, Zsolt; Szoboszlai, Norbert; Suskó, Emoke Klaudia; Mezei, Pál; György, Krisztina; Bencs, László

    2008-07-30

    A multi-element graphite furnace atomic absorption spectrometry (GFAAS) method was elaborated for the simultaneous determination of As, Cd, Cu, and Pb in wine samples of various sugar contents using the transversally heated graphite atomizer (THGA) with end-capped tubes and integrated graphite platforms (IGPs). For comparative GFAAS analyses, direct injection (i.e., dispensing the sample onto the IGP) and digestion-based (i.e., adding oxidizing agents, such as HNO(3) and/or H(2)O(2) to the sample solutions) methods were optimized with the application of chemical modifiers. The mixture of 5 microg Pd (applied as nitrate) plus 3 microg Mg(NO(3))(2) chemical modifier was proven to be optimal for the present set of analytes and matrix, it allowing the optimal 600 degrees C pyrolysis and 2200 degrees C atomization temperatures, respectively. The IGP of the THGA was pre-heated at 70 degrees C to prevent the sputtering and/or foaming of sample solutions with a high organic content, dispensed together with the modifier solution, which method also improved the reproducibility of the determinations. With the digestion-based method, the recovery ranged between 87 and 122%, while with the direct injection method it was between 96 and 102% for Cd, Cu, and Pb, whereas a lower, compromise recovery of 45-85% was realized for As. The detection limits (LODs) were found to be 5.0, 0.03, 1.2, and 0.8 microg l(-1) for As, Cd, Cu, and Pb, respectively. The characteristic mass (m(0)) data were 24 pg As, 1.3 pg Cd, 13 pg Cu, and 35 pg Pb. The upper limits of the linear calibration range were 100, 2, 100, and 200 microg l(-1) for As, Cd, Cu, and Pb, respectively. The precisions were not worse than 4.8, 3.1, 3.7, and 2.3% for As, Cd, Cu, and Pb, respectively. For arsenic, a higher amount of the modifier (e.g., 20 microg Pd plus 12 microg Mg(NO(3))(2)) could be recommended to overcome the interference from the presence of sulphate and phosphate in wines. Although this method increased the

  15. Determination of arsenic in diesel, gasoline and naphtha by graphite furnace atomic absorption spectrometry using microemulsion medium for sample stabilization.

    Science.gov (United States)

    Brandão, Geisamanda Pedrini; de Campos, Reinaldo Calixto; Luna, Aderval Severino; de Castro, Eustáquio Vinicius Ribeiro; de Jesus, Honério Coutinho

    2006-08-01

    A procedure for the determination of As in diesel, gasoline and naphtha at microg L(-1) levels by GFAAS is proposed. Sample stabilization was achieved by the formation of three component solutions prepared by mixing appropriate volumes of the samples propan-1-ol and nitric acid aqueous solution. This mixture resulted in a one-phase medium, which was indefinitely stable. No changes in the analyte signals were observed over several days in spiked samples, proving long-term stabilization ability. The use of conventional (Pd) and permanent (Ir) modification was investigated and the former was preferred. Central composite design multivariate optimization defined the optimum microemulsion composition as well as the temperature program. In this way, calibration using aqueous analytical solutions was possible, since the same sensitivity was observed in the investigated microemulsion media and in 0.2% v/v HNO(3). Coefficients of correlation larger than 0.999 and an As characteristic mass of 22 pg were observed. Recoveries (n=4) obtained from spiked samples were 98+/-4, 99+/-3 and 103+/-5%, and the limits of detection in the original samples were 1.8, 1.2 and 1.5 microg L(-1) for diesel, gasoline and naphtha, respectively. Validation was performed by the analysis of a set of commercial samples by independent comparative procedures. No significant difference (Student's t-test, pnaphtha, equivalent to a sample throughput of 7 h(-1) for diesel and 10 h(-1) for gasoline and naphtha.

  16. Investigation of chemical modifiers for the determination of lead in fertilizers and limestone using graphite furnace atomic absorption spectrometry with Zeeman-effect background correction and slurry sampling

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Becker, Emilene M.; Dessuy, Morgana B. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil)

    2014-02-01

    In this work, chemical modifiers in solution (Pd/Mg, NH{sub 4}H{sub 2}PO{sub 4} and NH{sub 4}NO{sub 3}/Pd) were compared with permanent modifiers (Ir and Ru) for the determination of lead in fertilizer and limestone samples using slurry sampling and graphite furnace atomic absorption spectrometry with Zeeman-effect background correction. The analytical line at 283.3 nm was used due to some spectral interference observed at 217.0 nm. The NH{sub 4}H{sub 2}PO{sub 4} was abandoned due to severe spectral interference even at the 283.3-nm line. For Pd/Mg and NH{sub 4}NO{sub 3}/Pd the optimum pyrolysis and atomization temperatures were 900 °C and 1900 °C, respectively. For Ru and Ir, the integrated absorbance signal was stable up to pyrolysis temperatures of 700 °C and 900 °C, respectively, and up to atomization temperature of 1700 °C. The limit of detection (LOD) was 17 ng g{sup −1} using Pd/Mg and 29 ng g{sup −1} using NH{sub 4}NO{sub 3}/Pd. Among the permanent modifiers investigated, the LOD was 22 ng g{sup −1} Pb for Ir and 10 ng g{sup −1} Pb for Ru. The accuracy of the method was evaluated using the certified reference material NIST SRM 695. Although Ru provided lower LOD, which can be attributed to a lower blank signal, only the modifiers in solution showed concordant values of Pb concentration for the NIST SRM 695 and the most of analyzed samples. Moreover, the Pd/Mg modifier provided the highest sensitivity and for this reason it is more suitable for the determination of Pb in fertilizers samples in slurry; besides this it presented a better signal-to-noise ratio than NH{sub 4}NO{sub 3}/Pd. - Highlights: • Lead has been determined in fertilizers using slurry sampling GF AAS. • The mixture of palladium and magnesium nitrates was found to be the ideal chemical modifier. • Calibration could be carried out against aqueous standard solutions. • The proposed method is much faster than the EPA method, which includes sample digestion.

  17. Graphene oxide-TiO2 composite solid phase extraction combined with graphite furnace atomic absorption spectrometry for the speciation of inorganic selenium in water samples.

    Science.gov (United States)

    Zhang, Yanan; Chen, Beibei; Wu, Shaowei; He, Man; Hu, Bin

    2016-07-01

    In this paper, a method of graphene oxide (GO)-TiO2 composite solid phase extraction followed by graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the speciation of inorganic selenium in environmental waters. The adsorption behavior of inorganic Se(IV) and Se(VI) on the GO-TiO2(1:1) composite was investigated. It was found that Se(IV) was quantitatively retained on the GO-TiO2 composites within a wide pH range of 0.5-10, while Se(VI) was quantitatively adsorbed on GO-TiO2(1:1) composite at pH 0.5-2, and no obvious adsorption of Se(VI) within the pH range of 4-10 was found. By selecting pH 6.0, Se(IV) could be easily determined. After reduction of Se(VI), total Se was determined by the proposed method, and Se(VI) was calculated as the difference between the total Se and Se(IV). The factors affecting the separation/preconcentration of Se(IV) and Se(VI) were studied. Under the optimum conditions, the isothermal adsorption of Se(IV) on the GO-TiO2(1:1) composite fitted Langmuir model; a linear range over 0.1-12ngmL(-1) was obtained. The limit of detection (LOD) and precision of the method for Se(IV) was 0.04ngmL(-1) and 9.4% (cSe(IV)=0.5ngmL(-1), n=7), respectively. In order to verify the accuracy of the method, a standard water sample (GSBZ50031-94) was analyzed, and the determined value was in a good agreement to the certified value. The established method was applied to inorganic Se speciation in environmental water samples and the recovery of 87.4-102% was obtained for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Trace and Essential Elements Analysis in Cymbopogon citratus (DC.) Stapf Samples by Graphite Furnace-Atomic Absorption Spectroscopy and Its Health Concern

    Science.gov (United States)

    Anal, Jasha Momo H.

    2014-01-01

    Cymbopogon citratus (DC.) Stapf commonly known as lemon grass is used extensively as green tea and even as herbal tea ingredient across the world. Plants have the ability to uptake metals as nutrient from the soil and its environment which are so essential for their physiological and biochemical growth. Concentrations of these twelve trace elements, namely, Mg, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Mo, As, Cd, and Pb, are analysed by graphite furnace-atomic absorption spectroscopy (GF-AAS) and are compared with the permissible limits of FAO/WHO, ICMR, and NIH, USA, which are found to be within permissible limits. Toxic metals like As, Cd, and Pb, analysed are within the tolerable daily diet limit and at low concentration. PMID:25525430

  19. Trace and Essential Elements Analysis in Cymbopogon citratus (DC.) Stapf Samples by Graphite Furnace-Atomic Absorption Spectroscopy and Its Health Concern.

    Science.gov (United States)

    Anal, Jasha Momo H

    2014-01-01

    Cymbopogon citratus (DC.) Stapf commonly known as lemon grass is used extensively as green tea and even as herbal tea ingredient across the world. Plants have the ability to uptake metals as nutrient from the soil and its environment which are so essential for their physiological and biochemical growth. Concentrations of these twelve trace elements, namely, Mg, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Mo, As, Cd, and Pb, are analysed by graphite furnace-atomic absorption spectroscopy (GF-AAS) and are compared with the permissible limits of FAO/WHO, ICMR, and NIH, USA, which are found to be within permissible limits. Toxic metals like As, Cd, and Pb, analysed are within the tolerable daily diet limit and at low concentration.

  20. Trace and Essential Elements Analysis in Cymbopogon citratus (DC. Stapf Samples by Graphite Furnace-Atomic Absorption Spectroscopy and Its Health Concern

    Directory of Open Access Journals (Sweden)

    Jasha Momo H. Anal

    2014-01-01

    Full Text Available Cymbopogon citratus (DC. Stapf commonly known as lemon grass is used extensively as green tea and even as herbal tea ingredient across the world. Plants have the ability to uptake metals as nutrient from the soil and its environment which are so essential for their physiological and biochemical growth. Concentrations of these twelve trace elements, namely, Mg, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Mo, As, Cd, and Pb, are analysed by graphite furnace-atomic absorption spectroscopy (GF-AAS and are compared with the permissible limits of FAO/WHO, ICMR, and NIH, USA, which are found to be within permissible limits. Toxic metals like As, Cd, and Pb, analysed are within the tolerable daily diet limit and at low concentration.

  1. Reliability of graphite furnace atomic absorption spectrometry as ...

    African Journals Online (AJOL)

    Purpose: To evaluate the comparative efficiency of graphite furnace atomic absorption spectrometry (GFAAS) and hydride generation atomic absorption spectrometry (HGAAS) for trace analysis of arsenic (As) in natural herbal products (NHPs). Method: Arsenic analysis in natural herbal products and standard reference ...

  2. Reliability of graphite furnace atomic absorption spectrometry as ...

    African Journals Online (AJOL)

    Original Research Article. Reliability of graphite furnace atomic absorption spectrometry as alternative method for trace analysis of arsenic in natural medicinal products. Reem Saadi Khalid1*, ABM Helaluddin1, Reem Saadi Khalid1, Mohamed. Alaama1, Abdualrahman M Abdualkader1, Abdulrazak Kasmuri2 and Syed Atif.

  3. Pigment identification in artwork using graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Goltz, D M; Coombs, J; Marion, C; Cloutis, E; Gibson, J; Attas, M; Choo-Smith, L-P; Collins, C

    2004-06-17

    The use of a sampling technique is described for the identification of metals from inorganic pigments in paint. The sampling technique involves gently contacting a cotton swab with the painted surface to physically remove a minute quantity ( approximately 1-2mug) of pigment. The amount of material removed from the painted surface is invisible to the unaided eye and does not cause any visible effect to the painted surface. The cotton swab was then placed in a 1.5ml polystyrene beaker containing HNO(3) to extract pigment metals prior to analysis using graphite furnace atomic absorption spectrometry (GFAAS). GFAAS is well suited for identifying pigment metals since it requires small samples and many pigments consist of main group elements (e.g. Al) as well as transition metals (e.g. Zn, Fe and Cd). Using Cd (cadmium red) as the test element, the reproducibility of sampling a paint surface with the cotton swab was approximately 13% in either a water or oil medium. To test the feasibility of cotton sampling for pigment identification, samples were obtained from paintings (watercolour and oil) of a local collection. Raman spectra provided complementary information to the GFAAS, which together are essential for positive identification of some pigments. For example, GFAAS indicated the presence of Cu, but the Raman spectra positively identified the modern copper pigment phthalocyanine green (Cu(C(32)Cl(16)N(8)). Both Raman spectroscopy and GFAAS were useful for identifying ZnO as a white pigment.

  4. [Determination of stannum in urine by graphite furnace atomic absorption spectrometry].

    Science.gov (United States)

    Chen, Jiu; Wu, Shihua; Guo, Guanhao; Liu, Yimin

    2015-12-01

    To establish the method of graphite furnace atomic absorption spectrometry for the measurement of stannum in urine with calcium nitrate as the matrix modifier. Graphite tube was pretreated with calcium nitrate as the matrix modifier, the urine sample was diluted with 1% nitric acid and then direct injection was performed for these samples, and graphite furnace atomic absorption spectrometry was applied for measurement. The concentration of stannum in urine showed a good linear relationship within the range of 8.0~40.0 μg/L, with a correlation coefficient of 0.9981. The minimum detectable concentration was 0.72 μg/L, the degree of precision was 1.54%~6.69%, and the recovery rate was 99.23%~107.63%. This method can determine the content of stannum in urine accurately and rapidly, with a high sensitivity and a low cost.

  5. Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling.

    Science.gov (United States)

    dos Santos, Lisia M G; Welz, Bernhard; Araujo, Rennan G O; Jacob, Silvana do C; Vale, Maria Goreti R; Martens, Andreas; Gonzaga Martens, Irland B; Becker-Ross, Helmut

    2009-11-11

    A fast routine screening method for the simultaneous determination of cadmium and iron in bean and soil samples is proposed, using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for the determination of cadmium, and an adjacent secondary line, at 228.726 nm, for iron. Fourteen bean samples and 10 soil samples from nine states all over Brazil have been analyzed. The limits of detection (3 sigma, n = 10) were 2.0 microg kg(-1) for Cd and 4.5 mg kg(-1) for Fe. The relative standard deviation ranged from 4 to 7% for Cd and from 5 to 28% for Fe, which is usually acceptable for a screening method. The accuracy of the method has been confirmed by the analysis of two certified reference materials; the results were in agreement with the certified values at a 95% confidence interval.

  6. Study on Carbon Reduction of Guizhou Oolitic Hematite by Graphite in Muffle Furnace

    Science.gov (United States)

    Zhong, Zheng; Zhang, Jinzhu; Huang, Run; Li, Mingming; Wu, Jie

    2017-09-01

    Oolitic hematite is an important iron ore resource in China. The mixed powder of the Guizhou oolitic hematite, the graphite, and the calcium hydroxide was pressed in a cylindrical sample mold by a 16 Mpa pressure. The dried samples at 378K for 12h were reduced in a muffle furnace at the temperature between 1323K and 1473K. The microstructure and the metallization degree of the sample were studied by means of optical microscope and chemical analysis. The results show that the higher metallization degree of the Hezhang oolitic hematite was up to 80.2% at 1323K with carbon oxgen mole ratio 1.3, the metallization degree of the sample in a muffle furnace is lower than that in a microwave furrnace, the lower metallization degree of the sample should be concerned with that the redued metallic iron can be oxidized in the muffle furnace with the temperature cooling down very slowly.

  7. Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Elsheimer, H.N.; Fries, T.L.

    1990-01-01

    A method is described for the determination of total tin in silicate rocks utilizing a graphite furnace atomic absorption spectrometer with a stabilized-temperature platform furnace and Zeeman-effect background correction. The sample is decomposed by lithium metaborate fusion (3 + 1) in graphite crucibles with the melt being dissolved in 7.5% hydrochloric acid. Tin extractions (4 + 1 or 8 + 1) are executed on portions of the acid solutions using a 4% solution of tricotylphosphine oxide in methyl isobutyl ketone (MIBK). Ascorbic acid is added as a reducing agent prior to extraction. A solution of diammonium hydrogenphosphate and magnesium nitrate is used as a matrix modifier in the graphite furnace determination. The limit of detection is > 10 pg, equivalent to > 1 ??g l-1 of tin in the MIBK solution or 0.2-0.3 ??g g-61 in the rock. The concentration range is linear between 2.5 and 500 ??g l-1 tin in solution. The precision, measured as relative standard deviation, is < 20% at the 2.5 ??g l-1 level and < 7% at the 10-30 ??g l-1 level of tin. Excellent agreement with recommended literature values was found when the method was applied to the international silicate rock standards BCR-1, PCC-1, GSP-1, AGV-1, STM-1, JGb-1 and Mica-Fe. Application was made to the determination of tin in geological core samples with total tin concentrations of the order of 1 ??g g-1 or less.

  8. Chemometric evaluation of Cd, Co, Cr, Cu, Ni (inductively coupled plasma optical emission spectrometry) and Pb (graphite furnace atomic absorption spectrometry) concentrations in lipstick samples intended to be used by adults and children.

    Science.gov (United States)

    Batista, Érica Ferreira; Augusto, Amanda dos Santos; Pereira-Filho, Edenir Rodrigues

    2016-04-01

    A method was developed for determining the concentrations of Cd, Co, Cr, Cu, Ni and Pb in lipstick samples intended to be used by adults and children using inductively coupled plasma optical emission spectrometry (ICP OES) and graphite furnace atomic absorption spectrometry (GF AAS) after treatment with dilute HNO3 and hot block. The combination of fractional factorial design and Desirability function was used to evaluate the ICP OES operational parameters and the regression models using Central Composite and Doehlert designs were calculated to stablish the best working condition for all analytes. Seventeen lipstick samples manufactured in different countries with different colors and brands were analyzed. Some samples contained high concentrations of toxic elements, such as Cr and Pb, which are carcinogenic and cause allergic and eczematous dermatitis. The maximum concentration detected was higher than the permissible safe limits for human use, and the samples containing these high metal concentrations were intended for use by children. Principal component analysis (PCA) was used as a chemometrics tool for exploratory analysis to observe the similarities between samples relative to the metal concentrations (a correlation between Cd and Pb was observed). Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

    Science.gov (United States)

    Krawczyk-Coda, Magdalena

    2017-03-01

    In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

  10. Persistent sample circulation microextraction combined with graphite furnace atomic absorption spectroscopy for trace determination of heavy metals in fish species marketed in Kermanshah, Iran and human health risk assessment.

    Science.gov (United States)

    Safari, Yahya; Karimaei, Mostafa; Sharafi, Kiomars; Arfaeinia, Hossein; Moradi, Masoud; Fattahi, Nazir

    2017-11-21

    The persistent sample circulation microextraction (PSCME) joined with the graphite furnace atomic absorption spectrometry (GFAAS) was developed as a high preconcentration technique for the determination of heavy metals in fish species. In this method, a few microliter of organic solvent (40.0 µl carbon tetrachloride) was transferred to the bottom of a conical sample cup. Then a 10.0 ml of aqueous solution transformed to fine droplets while passing through an organic solvent. At this stage, metal-ligand hydrophobic complex was extracted into the organic solvent. After extraction, 20 µl of extraction solvent was injected into the graphite tube using an auto-sampler. Under the optimum conditions, enrichment factors and enhancement factor were in the range of 180-240 and 155-214, respectively. The calibration curves were linear in the range of 0.03-200 µg kg-1 and the limits of detections (LODs) were in the range of 0.01-0.05 µg kg-1 . The Repeatability (intra-day) and reproducibility (inter-day) for 0.50 µg l-1 of Hg and 0.10 µg l-1 of Cd and Pb were in the range of 3.1-4.2% (n = 7) and 4.3-6.1% (n = 7), respectively. A potential human health risk assessment was conducted by calculating estimated weekly intake (EWI) of the metals from eating fish and comparison of these values with provisional tolerable weekly intake (PTWI) values. EWI data for the studied metals through fish consumption were lower than the PTWI values. This article is protected by copyright. All rights reserved.

  11. Determination of Ultra-trace Rhodium in Water Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point Extraction Using 2-(5-Iodo-2-Pyridylazo)-5-Dimethylaminoaniline as a Chelating Agent.

    Science.gov (United States)

    Han, Quan; Huo, Yanyan; Wu, Jiangyan; He, Yaping; Yang, Xiaohui; Yang, Longhu

    2017-03-24

    A highly sensitive method based on cloud point extraction (CPE) separation/preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection has been developed for the determination of ultra-trace amounts of rhodium in water samples. A new reagent, 2-(5-iodo-2-pyridylazo)-5-dimethylaminoaniline (5-I-PADMA), was used as the chelating agent and the nonionic surfactant TritonX-114 was chosen as extractant. In a HAc-NaAc buffer solution at pH 5.5, Rh(III) reacts with 5-I-PADMA to form a stable chelate by heating in a boiling water bath for 10 min. Subsequently, the chelate is extracted into the surfactant phase and separated from bulk water. The factors affecting CPE were investigated. Under the optimized conditions, the calibration graph was linear in the range of 0.1-6.0 ng/mL, the detection limit was 0.023 ng/mL for rhodium and relative standard deviation was 3.67% (c = 1.0 ng/mL, n = 11).The method has been applied to the determination of trace rhodium in water samples with satisfactory results.

  12. Cobalt internal standard for Ni to assist the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis.

    Science.gov (United States)

    de Babos, Diego Victor; Bechlin, Marcos André; Barros, Ariane Isis; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta; de Oliveira, Silvana Ruella

    2016-05-15

    A new method is proposed for the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS), employing direct solid sample analysis (DSS) and internal standardization (IS). Cobalt was used as internal standard to minimize matrix effects during Ni determinations, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9937. The performance of the method was checked by analysis of six plant certified reference materials, and the results for Mo and Ni were in agreement with the certified values (95% confidence level, t-test). Analysis was made of different types of plant materials used as renewable sources of energy, including sugarcane leaves, banana tree fiber, soybean straw, coffee pods, orange bagasse, peanut hulls, and sugarcane bagasse. The concentrations found for Mo and Ni ranged from 0.08 to 0.63 ng mg(-1) and from 0.41 to 6.92 ng mg(-1), respectively. Precision (RSD) varied from 2.1% to 11% for Mo and from 3.7% to 10% for Ni. Limits of quantification of 0.055 and 0.074 ng were obtained for Mo and Ni, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Effect of different precursors on generation of reference spectra for structural molecular background correction by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry: Determination of antimony in cosmetics.

    Science.gov (United States)

    Barros, Ariane Isis; Victor de Babos, Diego; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta

    2016-12-01

    Different precursors were evaluated for the generation of reference spectra and correction of the background caused by SiO molecules in the determination of Sb in facial cosmetics by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis. Zeolite and mica were the most effective precursors for background correction during Sb determination using the 217.581nm and 231.147nm lines. Full 2 3 factorial design and central composite design were used to optimize the atomizer temperature program. The optimum pyrolysis and atomization temperatures were 1500 and 2100°C, respectively. A Pd(NO 3 ) 2 /Mg(NO 3 ) 2 mixture was employed as the chemical modifier, and calibration was performed at 217.581nm with aqueous standards containing Sb in the range 0.5-2.25ng, resulting in a correlation coefficient of 0.9995 and a slope of 0.1548s ng -1 . The sample mass was in the range 0.15-0.25mg. The accuracy of the method was determined by analysis of Montana Soil (II) certified reference material, together with addition/recovery tests. The Sb concentration found was in agreement with the certified value, at a 95% confidence level (paired t-test). Recoveries of Sb added to the samples were in the range 82-108%. The limit of quantification was 0.9mgkg -1 and the relative standard deviation (n=3) ranged from 0.5% to 7.1%. From thirteen analyzed samples, Sb was not detected in ten samples (blush, eye shadow and compact powder); three samples (two blush and one eye shadow) presented Sb concentration in the 9.1-14.5mgkg -1 range. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Coprecipitation Technique for Preconcentration of Some Metal Ions prior to Graphite Furnace Atomic Absorption Spectrometric Determination

    OpenAIRE

    上田, 穣一

    1998-01-01

    Summary-for the preconcentration of trace ions in the graphite furnace atomic absorption spectrometric determination (GFAAS), a rapid and simple coprecipitation method which does not need the filtration

  15. Graphite Furnace Atomic Absorption Spectrometric Determination of Bismuth(III) after Coprecipitation with Hafnium Hydroxide

    OpenAIRE

    Ueda, Joichi; Takagi, Midori

    1990-01-01

    A method for the coprecipitation of bismuth(III) with hafnium hydroxide followed by a graphite-furnace atomic absorption spectrometric determination is described. Hafnium hydroxide coprecipitates quantitatively 0.05–3 μg of bismuth(III) from 50–400 cm3 of sample solution at pH 5.8–11.2. The presence of 2.5–50 mg of hafnium in 25 cm3 does not affect the atomic absorbance of bismuth(III). The calibration curve is linear for 0.05–3 μg of bismuth(III) in 25 cm3 and passes through the origin. Inte...

  16. Speciation of As(III) and As(V) in water samples by graphite furnace atomic absorption spectrometry after solid phase extraction combined with dispersive liquid-liquid microextraction based on the solidification of floating organic drop.

    Science.gov (United States)

    Shamsipur, Mojtaba; Fattahi, Nazir; Assadi, Yaghoub; Sadeghi, Marzieh; Sharafi, Kiomars

    2014-12-01

    A solid phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) method, using diethyldithiphosphate (DDTP) as a proper chelating agent, has been developed as an ultra preconcentration technique for the determination of inorganic arsenic in water samples prior to graphite furnace atomic absorption spectrometry (GFAAS). Variables affecting the performance of both steps were thoroughly investigated. Under optimized conditions, 100mL of As(ΙΙΙ) solution was first concentrated using a solid phase sorbent. The extract was collected in 2.0 mL of acetone and 60.0 µL of 1-undecanol was added into the collecting solvent. The mixture was then injected rapidly into 5.0 mL of pure water for further DLLME-SFO. Total inorganic As(III, V) was extracted similarly after reduction of As(V) to As(III) with potassium iodide and sodium thiosulfate and As(V) concentration was calculated by difference. A mixture of Pd(NO3)2 and Mg(NO3)2 was used as a chemical modifier in GFAAS. The analytical characteristics of the method were determined. The calibration graph was linear in the rage of 10-100 ng L(-1) with detection limit of 2.5 ng L(-1). Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 80 ng L(-1) of As(ΙΙΙ) were 6.8% and 7.5%, respectively. The method was successfully applied to speciation of As(III), As(V) and determination of the total amount of As in water samples and in a certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

  17. A New Cross-Shaped Graphite Furnace with Ballast Body for Reduction of Interferences in Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    A. A. Asweisi

    2010-01-01

    Full Text Available A new crossed graphite furnace for atomic absorption spectrometry (GFAAS was designed and installed in heated graphite atomizer (HGA500 combined with Perkin-Elmer spectrometer (AAS1100. The Tungsten ballast body was inserted inside one part of the crossed furnace in a way perpendicular to light path. The analyzed sample was injected manually on the ballast body inside the cross and pushed into the measuring zone using the original inner and additional purge gas. The sample was adsorbed strongly on the ballast and evaporated and transferred with different rates at different temperatures during the temperature program allowing the separation of analyte and matrix signals. Analysis of middle volatile element such as copper and manganese in standard urine sample (seronorm 2525 showed complete separation of analyte and background signals with good sensitivity and repeatability.

  18. Determination of total selenium in nutritional supplements and selenised yeast by Zeeman-effect graphite furnace atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Ekelund, J.

    1989-01-01

    A method for the determination of total selenium in nutritional supplements and selenised yeast is described. The samples were ashed in nitric acid. Hydrochloric acid was used to prevent precipitation of, in particular, iron salts. After appropriate dilutions, the selenium was determined by Zeeman......-effect background corrected graphite furnace atomic absorption spectrometry. A furnace ashing step at 1100 °C was necessary in order to obtain a total recovery of selenium when present in the organic form. Palladium nitrate-magnesium nitrate was used as a matrix modifier. Independent methods were used to determine...

  19. [Determination of trace cobalt in human urine by graphite furnace atomic absorption spectrometr].

    Science.gov (United States)

    Zhong, L X; Ding, B M; Jiang, D; Liu, D Y; Yu, B; Zhu, B L; Ding, L

    2016-05-20

    To establish a method to determine cobalt in human urine by graphite furnace atomic absorption spectrometry. Urine with 2% nitric acid diluted two-fold, to quantify the curve, graphite furnace atomic absorption spectrometric detection. Co was linear within 2.5~40.0 ng/ml with r>0.999. Spike experiment showed that Co received good recovery rate, which was 90.8%~94.8%. Intra-assay precisions were 3.2%~5.1% for Co, inter-assay precisions were 4.4%~5.2% for Co. The method by using graphite furnace atomic absorption spectrometr to determine urine Co was fast, accurate and with low matrix effect. It could meet the requirement in GBZ/T 210.5-2008.

  20. [Graphite furnace atomic absorption spectrometry for determination of thallium in blood].

    Science.gov (United States)

    Zhang, Q L; Gao, G

    2016-04-20

    Colloidal palladium was used as chemical modifier in the determination of blood thallium by graphite furnace atomic absorption spectrometry. Blood samples were precipitated with 5% (V/V)nitric acid, and then determined by GFAAS with colloidal palladium used as a chemical modifier. 0.2% (W/V)sodium chloride was added in the standard series to improve the matrix matching between standard solution and sample. The detection limit was 0.2 μg/L. The correlation coefficient was 0.9991. The recoveries were between 93.9% to 101.5%.The relative standard deviations were between 1.8% to 2.7%.The certified reference material of whole blood thallium was determined and the result was within the reference range Conclusion: The method is accurate, simple and sensitive, and it can meet the needs of detection thallium in blood entirely.

  1. Optimization of beryllium determination in biological materials by graphite furnace AAS

    Energy Technology Data Exchange (ETDEWEB)

    Nakagawa, Kiyoshi; Yonemoto, Tadashi; Iwasa, Aiko; Matsubara, Ikuko (Tokyo Women' s Medical Coll. (Japan))

    1994-07-01

    A method was optimized to enhance the sensitivity of graphite furnace atomic absorption spectrometry for the determination of beryllium in biological materials. Magnesium nitrate was added to the acid-digested sample solution, and a low-noise photomultiplier was utilized. The amplifier was operated at 10 times the ordinary amplification. Best results were obtained with a magnesium concentration of 10[sup -3] M when 50 [mu]l of the solution was injected and ashed at 1250degC for 30 s. Under these conditions, the matrix alkali salts are diminished to such an extent that background correction can be readily made, without impairing the beryllium sensitivity. The detection limit is 0.005 ppb (Be 0.25 pg). By this method a beryllium content of 0.50 ng/g (SD 0.04, n=12) was found in NIST Bovine Liver (SMR 1577). (author).

  2. DETERMINING BERYLLIUM IN DRINKING WATER BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROSCOPY

    Science.gov (United States)

    A direct graphite furnace atomic absorption spectroscopy method for the analysis of beryllium in drinking water has been derived from a method for determining beryllium in urine. Ammonium phosphomolybdate and ascorbic acid were employed as matrix modifiers. The matrix modifiers s...

  3. Method for the determination of cobalt from biological products with graphite furnace atomic absorption spectrometer

    Science.gov (United States)

    Zamfir, Oana-Liliana; Ionicǎ, Mihai; Caragea, Genica; Radu, Simona; Vlǎdescu, Marian

    2016-12-01

    Cobalt is a chemical element with symbol Co and atomic number 27 and atomic weight 58.93. 59 Co is the only stable cobalt isotope and the only isotope to exist naturally on Earth. Cobalt is the active center of coenzymes called cobalamin or cyanocobalamin the most common example of which is vitamin B12. Vitamin B12 deficiency can potentially cause severe and irreversible damage, especially to the brain and nervous system in the form of fatigue, depression and poor memory or even mania and psychosis. In order to study the degree of deficiency of the population with Co or the correctness of treatment with vitamin B12, a modern optoelectronic method for the determination of metals and metalloids from biological samples has been developed, Graphite Furnace - Atomic Absorption Spectrometer (GF- AAS) method is recommended. The technique is based on the fact that free atoms will absorb light at wavelengths characteristic of the element of interest. Free atoms of the chemical element can be produced from samples by the application of high temperatures. The system GF-AAS Varian used as biological samples, blood or urine that followed the digest of the organic matrix. For the investigations was used a high - performance GF-AAS with D2 - background correction system and a transversely heated graphite atomizer. As result of the use of the method are presented the concentration of Co in the blood or urine of a group of patient in Bucharest. The method is sensitive, reproducible relatively easy to apply, with a moderately costs.

  4. Method 200.12 - Determination of Trace Elements in Marine Waters by StabilizedTemperature Graphite Furnace Atomic Absorption

    Science.gov (United States)

    This method provides procedures for the determination of total recoverable elements by graphite furnace atomic absorption (GFAA) in marine waters, including estuarine, ocean and brines with salinities of up to 35 ppt.

  5. Graphite furnace atomic absorption spectrometric determination of cadmium after solid-liquid extraction with dithizone

    Directory of Open Access Journals (Sweden)

    Azizollah Nezhadali

    2009-08-01

    Full Text Available A method for the determination of trace amount of cadmium ion after preconcentration by extracting its dithizone complex into molten naphthalene was developed. Several experimental conditions such as pH of the solution, stirring time, the amounts of naphthalene, standing time and volume of the solution were optimized. Trace amount of cadmium ion in aqueous solution of sample was chelated with 5 mL of 0.001 M dithizone at pH 8. After addition of 0.15 g naphthalene, the solution was heated to about 85 oC and stirred (800 rpm for 2 min to reproduce the microcrystalline naphthalene. Cadmium ion was determined by a graphite furnace atomic absorption spectrometer. The interfering effects of diverse concomitant ions (cations and anions were investigated. Artificial sea water and a standard reference material (SRM were analyzed by this method. The sensitivity and detection limit of 1.2 ngL-1 and 1.5 ng L-1 were found, respectively.

  6. [Determination of trace gallium by graphite furnace atomic absorption spectrometry in urine].

    Science.gov (United States)

    Zhou, L Z; Fu, S; Gao, S Q; He, G W

    2016-06-20

    To establish a method for determination trace gallium in urine by graphite furnace atomic absorption spectrometry (GFAAS). The ammonium dihydrogen phosphate was matrix modifier. The temperature effect about pyrolysis (Tpyr) and atomization temperature were optimized for determination of trace gallium. The method of technical standard about within-run, between-run and recoveries of standard were optimized. The method showed a linear relationship within the range of 0.20~80.00 μg/L (r=0.998). The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 5.0, 10.0, 20.0 μg/L concentration levels were 2.1%~5.5% and 2.3%~3.0%. The detection limit was 0.06 μg/L. The recoveries of gallium were 98.2%~101.1%. This method is simple, low detection limit, accurate, reliable and reproducible. It has been applied for determination of trace gallium in urine samples those who need occupation health examination or poisoning diagnosis.

  7. Surfactant/oil/water system for the determination of selenium in eggs by graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ieggli, C.V.S. [Departamento de Quimica, Avenida Roraima, 1000, Universidade Federal de Santa Maria, CEP 97110-970, Santa Maria, RS (Brazil); Bohrer, D. [Departamento de Quimica, Avenida Roraima, 1000, Universidade Federal de Santa Maria, CEP 97110-970, Santa Maria, RS (Brazil)], E-mail: ndenise@quimica.ufsm.br; Noremberg, S.; Nascimento, P.C. do; Carvalho, L.M. de [Departamento de Quimica, Avenida Roraima, 1000, Universidade Federal de Santa Maria, CEP 97110-970, Santa Maria, RS (Brazil); Vieira, S.L.; Reis, R.N. [Faculdade de Agronomia, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 7712, CEP 90540-000, Porto Alegre (Brazil)

    2009-06-15

    An oil-in-water formulation has been optimized to determine trace levels of selenium in whole hen eggs by graphite furnace atomic absorption spectrometry. This method is simpler and requires fewer reagents when compared with other sample pre-treatment procedures. Graphite furnace atomic absorption spectrometric (GF AAS) measurement was carried out using standard addition calibration and Pd as a modifier. The precision, expressed as relative standard deviation, was better than 5% and the limit of detection was 1 {mu}g L{sup - 1}. The validation of the method was performed against a standard reference material Whole Egg Powder (RM 8415), and the measured Se corresponded to 95.2% of the certified value. The method was used for the determination of the Se level in eggs from hens treated with Se dietary supplements. Inorganic and organic Se sources were added to hen feed. The Se content of eggs was higher when hens were fed with organic Se compared to the other treatments. The proposed method, including sample emulsification for subsequent Se determination by GF AAS has proved to be sensitive, reproducible, simple and economical.

  8. DC graphite arc furnace, a simple system to reduce mixed waste volume

    Energy Technology Data Exchange (ETDEWEB)

    Wittle, J.K.; Hamilton, R.A.; Trescot, J. [and others

    1995-12-31

    The volume of low-level radioactive waste can be reduced by the high temperature in a DC Graphite Arc Furnace. This volume reduction can take place with the additional benefit of having the solid residue being stabilized by the vitrified product produced in the process. A DC Graphite Arc Furnace is a simple system in which electricity is used to generate heat to vitrify the material and thermally decompose any organic matter in the waste stream. Examples of this type of waste are protective clothing, resins, and grit blast materials produced in the nuclear industry. The various Department of Energy (DOE) complexes produce similar low-level waste streams. Electro-Pyrolysis, Inc. and Svedala/Kennedy Van Saun are engineering and building small 50-kg batch and up to 3,000 kg/hr continuous feed DC furnaces for the remediation, pollution prevention, and decontamination and decommissioning segments of the treatment community. This process has been demonstrated under DOE sponsorship at several facilities and has been shown to produce stable waste forms from surrogate waste materials.

  9. Application of factorial design and Doehlert matrix in the optimisation of instrumental parameters for direct determination of silicon in naphtha using graphite furnace atomic absorption spectrometry

    OpenAIRE

    Amaro, Joana Angélica de Azerêdo; Ferreira, Sergio Luis Costa

    2004-01-01

    p. 246 – 249 A method for direct determination of silicon in naphtha samples using graphite furnace atomic absorption spectrometry (GFAAS) is proposed. The optimisation of the instrumental conditions was multivariate using a fractional factorial design and Doehlert matrix. Firstly, the fractional factorial design was performed for preliminary evaluation of the significance of the factors, the factors chosen being: sample volume, atomisation temperature, pyrolysis time and pyrolysis temp...

  10. A versatile microcomputer interface and peripheral devices: An application in deuterium lamp background correction graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Gökmen, A.; Yalcin, S.

    1992-01-01

    A versatile interface card for Apple IIe computer and various peripheral devices are designed to control instruments which generates transient signals like in graphite furnace atomic spectrometer. The interface card consists of a multiplexed analog-to-digital converter, a digital-to-analog converter, and a timer/counter chip. The timer/counter chip with 16 built-in registers can be programmed in many modes which provides a time base for real-time measurements. A stepper motor runs under the control of timer/counter chip independent of computer. A light chopper connected to the stepper motor is controlled easily by computer. A dual high-voltage switch can modulate dc light sources under computer control. This system is applied to D2-lamp background correction graphite furnace atomic absorption spectrometer. The D2 lamp is chopped by a mechanical chopper driven by a stepper motor and a hollow cathode lamp is modulated electronically. The data acquisition program is written in machine language and synchronization between light sources and computer is provided by chopper position signal through the interrupts. A sampling rate of 16 during a signal period at 50-Hz chopping frequency is found to be the optimum value. A large number of data collected during atomization period is compressed in machine code. This saved storage space and analysis time.

  11. [Determination of indium in whole blood by graphite furnace atomic absorption spectrometry].

    Science.gov (United States)

    He, Juntao; Liu, Fen; Xiang, Yingping; Li, Zhimin

    2015-08-01

    To investigate the sensitization effect of different chemical modifiers in the determination of indium in whole blood by graphite furnace atomic absorption spectrometry, and to develop a new method for the determination of indium in whole blood. A mixture of 0.3% HNO3 (V/V) + 0.1% Triton X-100 (V/V) was used as a diluent, and a solution of 1 000 µg/ml Pd (NO3)2 + 3 000 µg/ml Mg (NO3)2 was used as modifier. After being diluted five times, the concentration of indium of the blood was directly determined by graphite furnace atomic absorption spectrometry. The detection limit of the method was 0.33 µg/L, the linear range was 0.33~100.00 µg/L, the relative standard deviation was 1.43%~2.65%, and the recovery rate was 98.3%~105.3%. The method is simple and fast and has high recovery and precision, and it is suitable for the determination of indium in whole blood.

  12. ESTIMATION OF MEASUREMENT UNCERTAINTY IN THE DETERMINATION OF Fe CONTENT IN POWDERED TONIC FOOD DRINK USING GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Harry Budiman

    2010-06-01

    Full Text Available The evaluation of uncertainty measurement in the determination of Fe content in powdered tonic food drink using graphite furnace atomic absorption spectrometry was carried out. The specification of measurand, source of uncertainty, standard uncertainty, combined uncertainty and expanded uncertainty from this measurement were evaluated and accounted. The measurement result showed that the Fe content in powdered tonic food drink sample was 569.32 µg/5g, with the expanded uncertainty measurement ± 178.20 µg/5g (coverage factor, k = 2, at confidende level 95%. The calibration curve gave the major contribution to the uncertainty of the final results.   Keywords: uncertainty, powdered tonic food drink, iron (Fe, graphite furnace AAS

  13. Determination of Chlorine in Milk via Molecular Absorption of SrCl Using High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-07-20

    Total chlorine in milk was determined via the molecular absorption of diatomic strontium monochloride at 635.862 nm using high-resolution continuum source graphite furnace atomic absorption spectrometry. The effects of coating the graphite furnace, using different modifiers, amount of molecule-forming element, and different calibrants were investigated and optimized. Chlorine concentrations in milk samples were determined in a Zr-coated graphite furnace using 25 μg of Sr as the molecule-forming reagent and applying a pyrolysis temperature of 600 °C and a molecule-forming temperature of 2300 °C. Linearity was maintained up to 500 μg mL(-1) of Cl. The method was tested by analyzing a certified reference wastewater. The results were in the uncertainty limits of the certified value. The limit of detection of the method was 1.76 μg mL(-1). The chlorine concentrations in various cow milk samples taken from the market were found in the range of 588-1472 mg L(-1).

  14. Determination of Copper by Graphite Furnace Atomic Absorption Spectrophotometry: A Student Exercise in Instrumental Methods of Analysis.

    Science.gov (United States)

    Williamson, Mark A.

    1989-01-01

    Discusses a student exercise which requires the optimizing of the charring and atomization temperatures by producing a plot of absorbance versus temperature for each temperature parameter. Notes that although the graphite furnace atomic absorption spectroscopy technique has widespread industrial use, there are no published, structured experiments…

  15. Multiphoton laser wave-mixing absorption spectroscopy for samarium using a graphite furnace atomizer

    Energy Technology Data Exchange (ETDEWEB)

    Maniaci, Michael J.; Tong, William G. E-mail: william.tong@sdsu.edu

    2004-07-30

    Nonlinear laser wave-mixing optical technique is presented as a sensitive atomic spectroscopic method for the analysis of rare earth elements using an unmodified commercially available graphite furnace (GF) atomizer. A simple nonplanar backward-scattering degenerate four-wave mixing optical arrangement offers sub-picogram detection sensitivity with sub-Doppler Lorentzian-broadened resolution. Nonlinear wave mixing is an unusually sensitive absorption-based optical method that offers both excellent detection sensitivity and sub-Doppler spectral resolution. A mass detection limit of 0.7 pg and a concentration detection limit of 70 pg/ml are determined for a rare earth element, samarium, using the 429.7-nm excitation line.

  16. Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

    Science.gov (United States)

    de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2016-09-14

    An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. ANALYSIS OF ENERGY EFFICIENCY OF BUTT END CONNECTIONS CONSTRUCTION OF SIDE BUS PACKAGES AND CURRENT FEEDERS OF GRAPHITIZATION FURNACE

    Directory of Open Access Journals (Sweden)

    D. S. Yarymbash

    2013-12-01

    Full Text Available The methods of the electrical parameter identification of the butt end bus connections of graphitization furnace current feeders with side bus packets basing on the conjugate three-dimensional mathematical models of electromagnetic and electro-thermal processes are presented. The finite element methods of solving partial derivatives vector equations systems in three-dimensional domain are used. The temperature dependences of the electro-physical properties and thermo-physical properties of the active materials and the external bus surface conditions of natural convection and radiation heat transfer are taken into account. The high accuracy and computational efficiency numerical calculations by using variations of the finite elements densities in the computational domain are produced. The finite elements densities in the domains of the magnetic field concentration are increased. The basic and new designs of butt end bus systems of AC graphitization furnace are considered. The calculations of geometric parameters of the bus conductors by using the equality criterion of active loss densities are presented. The currents, voltage drops, current density, electrical losses densities, active and inductive resistance of bus of side bus packages, butt end bus connections and graphite feeders are identified. The energy efficiency of butt end graphitization furnace electrical connections of different numbers of parallel buses is analyzed. The technical decisions to reduce weight, active and reactive power losses of bus butt end connections are substantiated.

  18. Determination of silicon and aluminum in silicon carbide nanocrystals by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Dravecz, Gabriella; Bencs, László; Beke, Dávid; Gali, Adam

    2016-01-15

    The determination of Al contaminant and the main component Si in silicon carbide (SiC) nanocrystals with the size-distribution of 1-8nm dispersed in an aqueous solution was developed using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS). The vaporization/atomization processes were investigated in a transversally heated graphite atomizer by evaporating solution samples of Al and Si preserved in various media (HCl, HNO3). For Si, the best results were obtained by applying a mixture of 5µg Pd plus 5µg Mg, whereas for Al, 10µg Mg (each as nitrate solution) was dispensed with the samples, but the results obtained without modifier were found to be better. This way a maximum pyrolysis temperature of 1200°C for Si and 1300°C for Al could be used, and the optimum (compromise) atomization temperature was 2400°C for both analytes. The Si and Al contents of different sized SiC nanocrystals, dispersed in aqueous solutions, were determined against aqueous (external) calibration standards. The correlation coefficients (R values) of the calibrations were found to be 0.9963 for Si and 0.9991 for Al. The upper limit of the linear calibration range was 2mg/l Si and 0.25mg/l Al. The limit of detection was 3µg/l for Si and 0.5µg/l for Al. The characteristic mass (m0) was calculated to be 389pg Si and 6.4pg Al. The Si and Al content in the solution samples were found to be in the range of 1.0-1.7mg/l and 0.1-0.25mg/l, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Development of a simple method for the determination of lead in lipstick using alkaline solubilization and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Soares, Aline Rodrigues; Nascentes, Clésia Cristina

    2013-02-15

    A simple method was developed for determining the total lead content in lipstick samples by graphite furnace atomic absorption spectrometry (GFAAS) after treatment with tetramethylammonium hydroxide (TMAH). Multivariate optimization was used to establish the optimal conditions of sample preparation. The graphite furnace heating program was optimized through pyrolysis and atomization curves. An aliquot containing approximately 50mg of the sample was mixed with TMAH and heated in a water bath at 60°C for 60 min. Using Nb as the permanent modifier and Pd as the chemical modifier, the optimal temperatures were 900°C and 1800°C for pyrolysis and atomization, respectively. Under optimum conditions, the working range was from 1.73 to 50.0 μg L(-1), with detection and quantification limits of 0.20 and 0.34 μg g(-1), respectively. The precision was evaluated under conditions of repeatability and intermediate precision and showed standard deviations of 2.37%-4.61% and 4.93%-9.75%, respectively. The % recovery ranged from 96.2% to 109%, and no significant differences were found between the results obtained using the proposed method and the microwave decomposition method for real samples. Lead was detected in 21 tested lipstick samples; the lead content in these samples ranged from 0.27 to 4.54 μg g(-1). Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Selective speciation of inorganic antimony on tetraethylenepentamine bonded silica gel column and its determination by graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Mendil, Durali; Bardak, Hilmi; Tuzen, Mustafa; Soylak, Mustafa

    2013-03-30

    A speciation system for antimony (III) and antimony (V) ions that based on solid phase extraction on tetraethylenepentamine bonded silica gel has been established. Antimony was determined by graphite furnace atomic absorption spectrometry (GF-AAS). Analytical conditions including pH, sample volume, etc., were studied for the quantitative recoveries of Sb (III) and Sb (V). Matrix effects on the recovery were also investigated. The recovery values and detection limit for antimony (III) at optimal conditions were found as >95% and 0.020 μg L(-1), respectively. Preconcentration factor was calculated as 50. The capacity of adsorption for the tetraethylenepentamine bonded silica gel was 7.9 mg g(-1). The validation was checked by analysis of NIST SRM 1573a Tomato laves and GBW 07605 Tea certified reference materials. The procedure was successfully applied to speciation of antimony in tap water, mineral water and spring water samples. Total antimony was determined in refined salt, unrefined salt, black tea, rice, tuna fish and soil samples after microwave digestion and presented enrichment method combination. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Sun, Mei; Wu, Qianghua

    2010-04-15

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL(-1). The relative standard deviation (n=7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin. 2009 Elsevier B.V. All rights reserved.

  2. Magnesium alloys and graphite wastes encapsulated in cementitious materials: Reduction of galvanic corrosion using alkali hydroxide activated blast furnace slag

    Energy Technology Data Exchange (ETDEWEB)

    Chartier, D., E-mail: david.chartier@cea.fr [Commissariat à l' Energie Atomique et aux Energies Alternatives, CEA, DEN, DTCD, SPDE, F-30207 Bagnols-sur-Cèze (France); Muzeau, B. [DEN-Service d’Etude du Comportement des Radionucléides (SECR), CEA, Université Paris-Saclay, F-91191, Gif-sur-Yvette (France); Stefan, L. [AREVA NC/D& S - France/Technical Department, 1 place Jean Millier 92084 Paris La Défense (France); Sanchez-Canet, J. [Commissariat à l' Energie Atomique et aux Energies Alternatives, CEA, DEN, DTCD, SPDE, F-30207 Bagnols-sur-Cèze (France); Monguillon, C. [DEN-Service d’Etude du Comportement des Radionucléides (SECR), CEA, Université Paris-Saclay, F-91191, Gif-sur-Yvette (France)

    2017-03-15

    Highlights: • Embedded in cement, magnesium is corroded by residual water present in porosity of the matrix. • Corrosion is enhanced by galvanic phenomenon when magnesium is in contact with graphite. • Galvanic corrosion of magnesium in contact with graphite debris is shown to be severe with ordinary Portland cement. • Galvanic corrosion is significantly lowered in high alkali medium such as sodium hydroxide. • Sodium hydroxide activated blast furnace slag is a convenient binder to embed magnesium. - Abstract: Magnesium alloys and graphite from spent nuclear fuel have been stored together in La Hague plant. The packaging of these wastes is under consideration. These wastes could be mixed in a grout composed of industrially available cement (Portland, calcium aluminate…). Within the alkaline pore solution of these matrixes, magnesium alloys are imperfectly protected by a layer of Brucite resulting in a slow corrosion releasing hydrogen. As the production of this gas must be considered for the storage safety, and the quality of wasteform, it is important to select a cement matrix capable of lowering the corrosion kinetics. Many types of calcium based cements have been tested and most of them have caused strong hydrogen production when magnesium alloys and graphite are conditioned together because of galvanic corrosion. Exceptions are binders based on alkali hydroxide activated ground granulated blast furnace slag (BFS) which are presented in this article.

  3. Determination of boron isotope ratios by high-resolution continuum source molecular absorption spectrometry using graphite furnace vaporizers

    Science.gov (United States)

    Abad, Carlos; Florek, Stefan; Becker-Ross, Helmut; Huang, Mao-Dong; Heinrich, Hans-Joachim; Recknagel, Sebastian; Vogl, Jochen; Jakubowski, Norbert; Panne, Ulrich

    2017-10-01

    Boron isotope amount ratios n(10B)/n(11B) have been determined by monitoring the absorption spectrum of boron monohydride (BH) in a graphite furnace using high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Bands (0 → 0) and (1 → 1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Clean and free of memory effect molecular spectra of BH were recorded. In order to eliminate the memory effect of boron, a combination of 2% (v/v) hydrogen gas in argon and 1% trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers was used. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, for the evaluated region of 437 nm, an accuracy of 0.15‰ is obtained as the average deviation from the isotope reference materials. Expanded uncertainties with a coverage factor of k = 2 range between 0.15 and 0.44‰. This accuracy and precision are compatible with those obtained by mass spectrometry for boron isotope ratio measurements.

  4. Standard test method for graphite furnace atomic absorption spectrometric determination of lead and cadmium extracted from ceramic foodware

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2000-01-01

    1.1 This test method covers procedures for using graphite furnace atomic absorption spectroscopy (GFAAS) to quantitatively determine lead and cadmium extracted by acetic acid at room temperature from the food-contact surface of foodware. The method is applicable to food-contact surfaces composed of silicate-based materials (earthenware, glazed ceramicware, decorated ceramicware, decorated glass, and lead crystal glass) and is capable of determining lead concentrations greater than 0.005 to 0.020 g/mL and cadmium concentrations greater than 0.0005 to 0.002 g/mL, depending on instrument design. 1.2 This test method also describes quality control procedures to check for contamination and matrix interference during GFAAS analyses and a specific sequence of analytical measurements that demonstrates proper instrument operation during the time period in which sample solutions are analyzed. 1.3 Cleaning and other contamination control procedures are described in this test method. Users may modify contamination cont...

  5. Fast and direct screening of copper in micro-volumes of distilled alcoholic beverages by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Ajtony, Zsolt; Laczai, Nikoletta; Dravecz, Gabriella; Szoboszlai, Norbert; Marosi, Áron; Marlok, Bence; Streli, Christina; Bencs, László

    2016-12-15

    HR-CS-GFAAS methods were developed for the fast determination of Cu in domestic and commercially available Hungarian distilled alcoholic beverages (called pálinka), in order to decide if their Cu content exceeds the permissible limit, as legislated by the WHO. Some microliters of samples were directly dispensed into the atomizer. Graphite furnace heating programs, effects/amounts of the Pd modifier, alternative wavelengths (e.g., Cu I 249.2146nm), external calibration and internal standardization methods were studied. Applying a fast graphite furnace heating program without any chemical modifier, the Cu content of a sample could be quantitated within 1.5min. The detection limit of the method is 0.03mg/L. Calibration curves are linear up to 10-15mg/L Cu. Spike-recoveries ranged from 89% to 119% with an average of 100.9±8.5%. Internal calibration could be applied with the assistance of Cr, Fe, and/or Rh standards. The accuracy of the GFAAS results was verified by TXRF analyses. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. Graphite furnace atomic absorption spectrophotometry--a novel method to quantify blood volume in experimental models of intracerebral hemorrhage.

    Science.gov (United States)

    Kashefiolasl, Sepide; Foerch, Christian; Pfeilschifter, Waltraud

    2013-02-15

    Intracerebral hemorrhage (ICH) accounts for 10% of all strokes and has a significantly higher mortality than cerebral ischemia. For decades, ICH has been neglected by experimental stroke researchers. Recently, however, clinical trials on acute blood pressure lowering or hyperacute supplementation of coagulation factors in ICH have spurred an interest to also design and improve translational animal models of spontaneous and anticoagulant-associated ICH. Hematoma volume is a substantial outcome parameter of most experimental ICH studies. We present graphite furnace atomic absorption spectrophotometric analysis (AAS) as a suitable method to precisely quantify hematoma volumes in rodent models of ICH. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. Magnesium alloys and graphite wastes encapsulated in cementitious materials: Reduction of galvanic corrosion using alkali hydroxide activated blast furnace slag.

    Science.gov (United States)

    Chartier, D; Muzeau, B; Stefan, L; Sanchez-Canet, J; Monguillon, C

    2017-03-15

    Magnesium alloys and graphite from spent nuclear fuel have been stored together in La Hague plant. The packaging of these wastes is under consideration. These wastes could be mixed in a grout composed of industrially available cement (Portland, calcium aluminate…). Within the alkaline pore solution of these matrixes, magnesium alloys are imperfectly protected by a layer of Brucite resulting in a slow corrosion releasing hydrogen. As the production of this gas must be considered for the storage safety, and the quality of wasteform, it is important to select a cement matrix capable of lowering the corrosion kinetics. Many types of calcium based cements have been tested and most of them have caused strong hydrogen production when magnesium alloys and graphite are conditioned together because of galvanic corrosion. Exceptions are binders based on alkali hydroxide activated ground granulated blast furnace slag (BFS) which are presented in this article. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Determination of platinum traces contamination by graphite furnace atomic absorption spectrometry after preconcentration by cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Chappuy, M. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Caudron, E., E-mail: eric.caudron@eps.aphp.fr [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France); Groupe de Chimie Analytique de Paris-Sud, EA 4041, IFR 141, School of Pharmacy, Univ Paris-Sud, 92296 Chatenay-Malabry (France); Bellanger, A. [Department of Pharmacy, Pitie-Salpetriere Hospital (Paris Public Hospital Authority), 47 boulevard de l' hopital, 75013 Paris (France); Pradeau, D. [Analytical Development Laboratory, Pharmaceutical Establishment of Paris Hospitals, 7 rue du Fer a Moulin, 75005 Paris (France)

    2010-04-15

    A simple and sensitive method is described for the determination of platinum surface contamination originating from cisplatin, carboplatin and oxaliplatin. Following extraction from swabs and preconcentration with the cloud point extraction (CPE) method, detection was by graphite furnace atomic absorption spectrometry (GFAAS). After desorption of platinum compounds from the swab, CPE involved on preconcentration of platinum in aqueous solution with diethyldithiocarbamate (DDTC) as chelating agent and Triton X-114 as extraction medium. DDTC is not only a chelating agent, but may also be a good candidate for the inactivation of platinum compounds. DDTC is recommended by the Word Health Organization (WHO) for the destruction of platinum-based anticancer drugs. The main factors affecting CPE efficiency, pH of the sample solution, concentrations of DDTC and Triton X-114, equilibration temperature and incubation time, were evaluated in order to enhance sensitivity of the method. The desorption of platinum compounds from the swab was investigated in parallel. Since platinum is bound to DDTC, it must exchange with copper in order to enhance platinum atomizing by GFAAS. A preconcentration factor of 29 was obtained for 10 mL of a platinum solution at 10 {mu}g mL{sup -1}. In optimal conditions, the limit of detection was 0.2 ng mL{sup -1}, corresponding to 2.0 ng of platinum metal on the swab. Absorbance was linear between 0.7 and 15 ng mL{sup -1}. The proposed method was applied for the determination of surface contamination by platinum compounds with correct results.

  9. Speciation of platinum in blood plasma and urine by micelle-mediated extraction and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Mortada, Wael I; Hassanien, Mohammed M; El-Asmy, Ahmed A

    2013-10-01

    A highly sensitive and selective technique for the speciation of platinum by cloud point extraction prior to determination by graphite furnace atomic absorption spectrometry (GFAAS) was described. The separation of Pt(II) from Pt(IV) was performed in the presence of 4-(p-chlorophenyl)-1-(pyridin-2-yl)thiosemicarbazide (HCPTS) as chelating agent and Triton X-114 as a non-ionic surfactant. The extraction of Pt(II)-HCPTS complex needs temperature higher than the cloud point temperature of Triton X-114 and pH = 7, while Pt(IV) remains in the aqueous phase. The Pt(II) in the surfactant phase was analyzed by GFAAS, and the concentration of Pt(IV) was calculated by subtraction of Pt(II) from total platinum which was directly determined by GFAAS. The effect of pH, concentration of chelating agent, surfactant, and equilibration temperature were investigated. An enrichment factor of 42 was obtained for the preconcentration of Pt(II) with 50 mL solution. Under the optimum experimental conditions, the calibration curve was linear up to 30 μgL(-1) with detection limit of 0.08 μgL(-1) and the relative standard deviation was 1.8%. No considerable interference was observed due to the presence of coexisting anions and cations. The accuracy of the results was verified by analyzing different spiked samples (tap water, blood plasma and urine). The proposed method was applied to the speciation analysis of Pt in blood plasma and urine with satisfactory results. Copyright © 2013 Elsevier GmbH. All rights reserved.

  10. Cadmium, copper, lead, and zinc determination in precipitation: A comparison of inductively coupled plasma atomic emission spectrometry and graphite furnace atomization atomic absorption spectrometry

    Science.gov (United States)

    Reddy, M.M.; Benefiel, M.A.; Claassen, H.C.

    1987-01-01

    Selected trace element analysis for cadmium, copper, lead, and zinc in precipitation samples by inductively coupled plasma atomic emission Spectrometry (ICP) and by atomic absorption spectrometry with graphite furnace atomization (AAGF) have been evaluated. This task was conducted in conjunction with a longterm study of precipitation chemistry at high altitude sites located in remote areas of the southwestern United States. Coefficients of variation and recovery values were determined for a standard reference water sample for all metals examined for both techniques. At concentration levels less than 10 micrograms per liter AAGF analyses exhibited better precision and accuracy than ICP. Both methods appear to offer the potential for cost-effective analysis of trace metal ions in precipitation. ?? 1987 Springer-Verlag.

  11. Direct determination of particulate elements in edible oils and fats using an ultrasonic slurry sampler with graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    van Dalen, Gerard; de Galan, Leo

    1994-12-01

    Through the use of an ultrasonic slurry mixer, graphite furnace atomic absorption spectrometry (GFAAS) can be applied for the fully automated determination of particulate iron and nickel in edible oils and fats. The unsupervised ultrasonic slurry autosampler yields the same accuracy and somewhat better precision than the much more laborious manual GFAAS method.

  12. Performance of permanent iridium modifier in the presence of corrosive matrix in graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Piascik, M.; Bulska, E. [Univ. of Warsaw (Poland). Dept. of Chemistry

    2001-12-01

    The influence of up to 16% HNO{sub 3}, 28% HCl, and the mixture of both acids in aqua regia on the analytical performance of electrodeposited modifiers (Ir or Ir+Pd) was evaluated and discussed. Cadmium was used as an example of volatile elements often determined by graphite furnace atomic absorption spectrometry (GF AAS). In the presence of HCl, the maximum pyrolysis temperature that could be applied was found to be 600 C. In the presence of HNO{sub 3} and aqua regia, both modifiers stabilized cadmium up to 800 C. The long-term performance of electrodeposited Ir or Ir+Pd was not influenced by mineral acids; moreover the tube lifetime was significantly prolonged compared with a non-modified tube. (orig.)

  13. Method for processing aluminum spent potliner in a graphite electrode ARC furnace

    Science.gov (United States)

    O'Connor, William K.; Turner, Paul C.; Addison, Gerald W.

    2002-12-24

    A method of processing spent aluminum pot liner containing carbon, cyanide compositions, fluorides and inorganic oxides. The spent aluminum pot liner is crushed iron oxide is added to form an agglomerated material. The agglomerated material is melted in an electric arc furnace having the electrodes submerged in the molten material to provide a reducing environment during the furnace operation. In the reducing environment, pot liner is oxidized while the iron oxides are reduced to produce iron and a slag substantially free of cyanide compositions and fluorides. An off-gas including carbon oxides and fluorine is treated in an air pollution control system with an afterburner and a scrubber to produce NaF, water and a gas vented to the atmosphere free of cyanide compositions, fluorine and CO.

  14. Investigation of chemical modifiers for the direct determination of arsenic in fish oil using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Pereira, Éderson R; de Almeida, Tarcísio S; Borges, Daniel L G; Carasek, Eduardo; Welz, Bernhard; Feldmann, Jörg; Campo Menoyo, Javier Del

    2016-04-01

    High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Fast arsenic speciation in water by on-site solid phase extraction and high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Mihucz, Victor G.; Bencs, László; Koncz, Kornél; Tatár, Enikő; Weiszburg, Tamás; Záray, Gyula

    2017-02-01

    A method of high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS), combined with on-site separation/solid phase extraction (SPE) has been developed for the speciation of inorganic As (iAs) in geothermal and drinking water samples. The HR-CS-GFAAS calibration curves were linear up to 200 μg/L As, but using second order polynomial fitting, accurate calibration could be performed up to 500 μg/L. It has been demonstrated that sample pH should not be higher than 8 for an accurate speciation of As(V) with a recovery of ≈ 95%. Geothermal water had fairly high salt content (≈ 2200 mg/L) due to the presence of chlorides and sulfates at mg/L levels. Therefore, a two-fold dilution of these types of samples before SPE is recommended, especially, for total As determinations, when the As concentration is as high as 400 μg/L. For drinking water, sampled from public wells with records of As concentrations higher than the 10 μg/L in the past, the reduction of As contamination below the WHO's health limit value could be observed. However, the electrical conductivity was close to 2500 μS/cm, i.e., the guideline limit for drinking water, which was due to their higher chloride content. The proposed fit-for-purpose SPE-HR-CS-GFAAS method could be a candidate for screening drinking water quality.

  16. Ultrasound-Assisted Emulsification Microextraction Based on Solidification Floating Organic Drop Trace Amounts of Manganese Prior to Graphite Furnace Atomic Absorption Spectrometry Determination

    Science.gov (United States)

    Mohadesi, Alireza; Falahnejad, Masoumeh

    2012-01-01

    In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn+2 at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50–10.0 ng mL−1 with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL−1 was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples. PMID:22645504

  17. RAPID AND SENSITIVE DETERMINATION OF PALLADIUM USING HOMOGENEOUS LIQUID-LIQUID MICROEXTRACTION VIA FLOTATION ASSISTANCE FOLLOWED BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Mohammad Rezaee

    2015-05-01

    Full Text Available A method for the determination of trace amounts of palladium was developed using homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA followed by graphite furnace atomic absorption spectrometry (GFAAS. Ammonium pyrrolidine dithiocarbamate (APDC was used as a complexing agent. This was applied to determine palladium in three types of water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added to the extraction cell which contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Parameters affecting extraction efficiency were investigated and optimized. Under the optimum conditions, the calibration graph was linear in the range of 1.0-200 µg L-1 with a limit of detection of 0.3 µg L-1. The performance of the method was evaluated for the extraction and determination of palladium in water samples and satisfactory results were obtained. In order to verify the accuracy of the approach, the standard addition method was applied for the determination of palladium in spiked synthetic samples and satisfactory results were obtained.

  18. Determination of sulfur in human hair using high resolution continuum source graphite furnace molecular absorption spectrometry and its correlation with total protein and albumin

    Science.gov (United States)

    Ozbek, Nil; Baysal, Asli

    2017-04-01

    Human hair is a valuable contributor for biological monitoring. It is an information storage point to assess the effects of environmental, nutritional or occupational sources on the body. Human proteins, amino acids or other compounds are among the key components to find the sources of different effects or disorders in the human body. Sulfur is a significant one of these compounds, and it has great affinity to some metals and compounds. This property of the sulfur affects the human health positively or negatively. In this manuscript, sulfur was determined in hair samples of autistic and age-match control group children via molecular absorption of CS using a high-resolution continuum source graphite furnace atomic absorption spectrometer. For this purpose, hair samples were appropriately washed and dried at 75 °C. Then samples were dissolved in microwave digestion using HNO3 for sulfur determination. Extraction was performed with HCl hydrolysation by incubation for 24 h at 110 °C for total protein and albumin determination. The validity of the method for the sulfur determination was tested using hair standard reference materials. The results were in the uncertainty limits of the certified values at 95% confidence level. Finally correlation of sulfur levels of autistic children's hair with their total protein and albumin levels were done.

  19. Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometric for selenium speciation in foods and beverages.

    Science.gov (United States)

    Tuzen, Mustafa; Pekiner, Ozlem Zeynep

    2015-12-01

    A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. Optimization and validation of a methodology to determine total arsenic, As(III and As(V, in water samples, through graphite furnace atomic absorption spectrometry Otimização e validação de metodologia de determinação de arsênio total, As(III e As(V, em amostras de água por espectrometria de absorção atômica com forno de grafite

    Directory of Open Access Journals (Sweden)

    Lisia Maria Gobbo Santos

    2009-03-01

    Full Text Available The Graphite furnace atomic absorption spectrometry (GF AAS was the technique chosen by the inorganic contamination laboratory (INCQ/ FIOCRUZ to be validated and applied in routine analysis for arsenic detection and quantification. The selectivity, linearity, sensibility, detection, and quantification limits besides accuracy and precision parameters were studied and optimized under Stabilized Temperature Platform Furnace (STPF conditions. The limit of detection obtained was 0.13 µg.L-1 and the limit of quantification was 1.04 µg.L-1, with an average precision, for total arsenic, less than 15% and an accuracy of 96%. To quantify the chemical species As(III and As(V, an ion-exchange resin (Dowex 1X8, Cl- form was used and the physical-chemical parameters were optimized resulting in a recuperation of 98% of As(III and of 90% of As(V. The method was applied to groundwater, mineral water, and hemodialysis purified water samples. All results obtained were lower than the maximum limit values established by the legal Brazilian regulations, in effect, 50, 10, and 5 µg.L-1 para As total, As(III e As(V, respectively. All results were statistically evaluated.A técnica de espectrometria de absorção atômica com forno de grafite (GF AAS foi a técnica escolhida pelo laboratório de contaminantes inorgânicos do Instituto Nacional de Controle de Qualidade em Saúde (INCQS/FIOCRUZ para ser validada e aplicada em análises de rotina para detecção e quantificação de arsênio. Os parâmetros de validação seletividade, linearidade, sensibilidade, limite de detecção e quantificação, exatidão e precisão foram estudados e otimizados usando as condições STPF (Stabilized Temperature Platform Furnace. Os resultados encontrados apresentaram limites de detecção 0,13 µg.L-1 e quantificação de 1,04 µg.L-1, uma precisão média para arsênio total inferior a 15% e uma exatidão de 96%. Para quantificar as espécies químicas As(III e As(V, utilizamos

  1. Testing of Small Graphite Samples for Nuclear Qualification

    Energy Technology Data Exchange (ETDEWEB)

    Julie Chapman

    2010-11-01

    Accurately determining the mechanical properties of small irradiated samples is crucial to predicting the behavior of the overal irradiated graphite components within a Very High Temperature Reactor. The sample size allowed in a material test reactor, however, is limited, and this poses some difficulties with respect to mechanical testing. In the case of graphite with a larger grain size, a small sample may exhibit characteristics not representative of the bulk material, leading to inaccuracies in the data. A study to determine a potential size effect on the tensile strength was pursued under the Next Generation Nuclear Plant program. It focuses first on optimizing the tensile testing procedure identified in the American Society for Testing and Materials (ASTM) Standard C 781-08. Once the testing procedure was verified, a size effect was assessed by gradually reducing the diameter of the specimens. By monitoring the material response, a size effect was successfully identified.

  2. Graphite

    Science.gov (United States)

    Robinson, Gilpin R.; Hammarstrom, Jane M.; Olson, Donald W.; Schulz, Klaus J.; DeYoung, John H.; Seal, Robert R.; Bradley, Dwight C.

    2017-12-19

    Graphite is a form of pure carbon that normally occurs as black crystal flakes and masses. It has important properties, such as chemical inertness, thermal stability, high electrical conductivity, and lubricity (slipperiness) that make it suitable for many industrial applications, including electronics, lubricants, metallurgy, and steelmaking. For some of these uses, no suitable substitutes are available. Steelmaking and refractory applications in metallurgy use the largest amount of produced graphite; however, emerging technology uses in large-scale fuel cell, battery, and lightweight high-strength composite applications could substantially increase world demand for graphite.Graphite ores are classified as “amorphous” (microcrystalline), and “crystalline” (“flake” or “lump or chip”) based on the ore’s crystallinity, grain-size, and morphology. All graphite deposits mined today formed from metamorphism of carbonaceous sedimentary rocks, and the ore type is determined by the geologic setting. Thermally metamorphosed coal is the usual source of amorphous graphite. Disseminated crystalline flake graphite is mined from carbonaceous metamorphic rocks, and lump or chip graphite is mined from veins in high-grade metamorphic regions. Because graphite is chemically inert and nontoxic, the main environmental concerns associated with graphite mining are inhalation of fine-grained dusts, including silicate and sulfide mineral particles, and hydrocarbon vapors produced during the mining and processing of ore. Synthetic graphite is manufactured from hydrocarbon sources using high-temperature heat treatment, and it is more expensive to produce than natural graphite.Production of natural graphite is dominated by China, India, and Brazil, which export graphite worldwide. China provides approximately 67 percent of worldwide output of natural graphite, and, as the dominant exporter, has the ability to set world prices. China has significant graphite reserves, and

  3. Ultrasound-assisted emulsification-microextraction combined with graphite furnace atomic absorption spectrometry for the determination of trace lead in water

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Hongmei; Zhang, Yu; Qiu, Bocheng; Li, Wenhua [College of Science, Nanjing Agricultural University, Nan Jing (China)

    2012-04-15

    The ultrasound-assisted emulsification-microextraction (USAEME) method was combined with graphite furnace atomic absorption spectrometry (GFAAS) for the determination of trace Pb using dithizone (H{sup 2}DZ) as chelating reagent. Some effective parameters influenced the detection and microextraction, such as ashing temperature and atomization temperature, pH, extraction solvent, sample volume, extraction time, and extraction temperature were selected and optimized. After extraction, the calibration curves for Pb was in the concentration range of 0.1-10 ng mL{sup -1}, and the linear equation was y = 0.097 x + 0.023 (R = 0.99). Under the optimized conditions, the detection limit of the method was 20 pg mL{sup -1} with an enrichment factor of 70 and the relative standards deviation (RSD) for seven determinations of 1 ng mL{sup -1} Pb was 11%. The proposed method was successfully applied to determine trace Pb in Yueya Lake water, pond water, and spiked samples. Furthermore, a certified reference material of Environment Water (GBW08607) was analyzed and the determined value was in good agreement with the certified value, which showed the accuracy, recovery, and applicability of the reported method. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  4. Determination of total selenium in pharmaceutical and herbal supplements by hydride generation and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Kazi, Tasneem G; Kolachi, Nida F; Afridi, Hassan I; Brahman, Kapil Dev; Shah, Faheem

    2014-01-01

    The total selenium (Se) was determined in herbal and pharmaceutical supplements used for liver diseases. The total Se contents were determined in different pharmaceutical and herbal supplements by hydride generation atomic absorption spectrometry (HGAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after microwave-assisted acid digestion. The accuracy of the techniques was evaluated by using certified reference material and the standard addition method. The recoveries of total Se were 99.4 and 99.0% for HGAAS and GFAAS, respectively. The precision of the techniques expressed as RSD were 2.34 and 4.54% for HGAAS and GFAAS measurements, respectively. The LOD values for HGAAS and GFAAS were 0.025 and 0.052 pglg, respectively. The concentrations of Se in pharmaceutical and herbal supplements were found in the range of 19.2-53.8 and 25.0-42.5 pg/g, respectively, corresponding to 35-76% and 45-76% of the total recommended dose of Se for adults.

  5. A simple and selective approach for determination of trace Hg(II) using electromembrane extraction followed by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Kamyabi, Mohammad Ali; Aghaei, Ali

    2017-02-01

    The present study proposes the determination of trace Hg(II) using electromembrane extraction followed by graphite furnace atomic absorption spectrometry (GFAAS). Hg(II) migrated from 5 mL of an aqueous donor phase across a thin layer of supported liquid membrane, immobilized inside pores of a hollow fiber, into 10 μL of an acidic acceptor phase present inside the lumen of the fiber. The final analysis of the extracted Hg(II) performed using GFAAS (350 °C and 1400 °C for the ashing and atomization temperatures, respectively). Under optimal conditions, Hg(II) was effectively extracted with recoveries in the range of 41-43%, which corresponded to enrichment factors in the range of 102-108. The calibration curve was investigated in the range of 0.5-10 μg/L and a good linearity was achieved with a coefficient factor of 0.998. Detection limit (3σ) was found to be 0.5 μg/L and repeatability for 5 replicate determinations of three different concentration level of Hg(II) were found to be within the range of 6.2-7.1%. The reliability of the proposed method was examined by analyzing different real waters samples.

  6. Simultaneous determination of rhodium and ruthenium by high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Zambrzycka-Szelewa, Elżbieta; Lulewicz, Marta; Godlewska-Żyłkiewicz, Beata

    2017-07-01

    In the present paper a fast, simple and sensitive analytical method for simultaneous determination of rhodium and ruthenium by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) was developed. Among six pairs of absorption atomic lines of Rh and Ru, which are close enough to enable their simultaneous detection, two pairs were selected for further studies. Best results were obtained for measurements of the resonance line of rhodium at 343.489 nm and the adjacent secondary line of ruthenium at 343.674 nm (23% intensity of this line). For evaluated lines, the absorbance values were obtained using three pixels. The pyrolysis and atomization temperatures were 1200 °C and 2600 °C, respectively. Under these conditions the limits of detection achieved for Rh and Ru were found to be 1.0 μg L- 1 and 1.9 μg L- 1, respectively. The characteristic mass was 12.9 pg for Rh and 71.7 pg for Ru. Repeatability of the results expressed as a relative standard deviation was typically below 6%. The trueness of the method was confirmed by analysis of the certified reference material - platinum ore (SARM 76). The recovery of Rh and Ru from the platinum ore was 93.0 ± 4.6% and 90.1 ± 2.5%, respectively. The method was successfully applied to the direct simultaneous determination of trace amounts of rhodium and ruthenium in spiked river water, road runoff, and municipal sewage. Separation of interfering matrix on cation exchange resin was required before analysis of road dust and tunnel dust (CW-7) by HR-CS GFAAS.

  7. Trace determination of lead in lipsticks and hair dyes using microwave-assisted dispersive liquid-liquid microextraction and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Sharafi, K; Fattahi, N; Pirsaheb, M; Yarmohamadi, H; Fazlzadeh Davil, M

    2015-10-01

    A novel microwave-assisted dispersive liquid-liquid microextraction (MADLLME) technique according to the solidification of a floating organic droplet (SFO) and graphite furnace atomic absorption spectrometry (GFAAS) used for the extraction and determination of lead ions in lipsticks and hair dyes made in different countries. Lipstick and hair dye samples of different brands and colours were collected from local market in Kermanshah, Iran. After sample treatment with microwave-assisted acid digestion, an appropriate mixture of acetone, 1-undecanol and diethyl dithiophosphoric acid was injected rapidly into the aqueous sample containing lead ions, and as a result, cloudy mixture was formed. After centrifugation, the test tube was cooled for few minutes. The solidified 1-undecanol on top of the solution was transferred into a suitable vial and injected into the analytical instrument. Under the optimum experimental conditions (extraction solvent: 30 μL of 1-undecanol; disperser solvent: 500 μL of acetone; ligand concentration: 0.15% (v/v); pH: ~1.5 and without salt added), the enhancement factor of 96 was obtained. The calibration graphs were linear in the range of 0.3-50 μg kg(-1) with a correlation coefficient (r(2) ) more than 0.995. The detection limit was 0.1 μg kg(-1) . Consequently, the developed method was successfully applied to extract and determine lead ions in the lipsticks and hair dyes, and favourable results were obtained. The proposed method which applied in cosmetics showed excellent relative recoveries (90-109.7%) with relative standard deviations market is far below the recommended limits as applied in Germany (20 mg kg(-1) ) and Canada (10 mg kg(-1) ) and confirmed that very low levels of lead are technically available in the final cosmetic products. © 2015 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

  8. Speciation analysis of volatile and non-volatile vanadium compounds in Brazilian crude oils using high-resolution continuum source graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lepri, Fabio G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Welz, Bernhard [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil)]. E-mail: welz@qmc.ufsc.br; Borges, Daniel L.G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Silva, Alessandra F. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Vale, Maria Goreti R. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Heitmann, Uwe [ISAS - Institute of Analytical Sciences, Department Berlin, Albert-Einstein-Str. 9, 12489 Berlin (Germany)

    2006-02-03

    A method is proposed that makes possible determining total and 'thermally stable' vanadium in crude oil without prior separation, and to calculate 'volatile' vanadium by difference. The volatile fraction is believed to be largely vanadyl porphyrine complexes. The method is based on the unsurpassed background correction capability of high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS), which allows pyrolysis temperatures as low as 300 deg. C to be used. The samples were prepared as oil-in-water emulsions, and aqueous standards emulsified in the same way were used for calibration. Total vanadium has been determined using a pyrolysis temperature of 400 deg. C, and 'thermally stable' vanadium using a pyrolysis temperature of 800 deg. C. The content of total vanadium in 12 Brazilian crude oil samples was found to be between less than 0.04 and about 30 mg kg{sup -1}. The volatile fraction was between 5 and 51% of the total content, and there was no correlation between the total and the volatile vanadium content. The limits of detection and quantification were 0.04 and 0.12 mg kg{sup -1} of V in crude oil, respectively, based on a mass of 2 g of oil in 10 mL of emulsion. The precision was better than 4% at the 3 mg kg{sup -1} level and better than 1.5% at the 30 mg kg{sup -1} level of V in crude oil.

  9. Determination of Pb (Lead), Cd (Cadmium), Cr (Chromium), Cu (Copper), and Ni (Nickel) in Chinese tea with high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Zhong, Wen-Si; Ren, Ting; Zhao, Li-Jiao

    2016-01-01

    The contents of lead, cadmium, chromium, copper, and nickel were determined in 25 tea samples from China, including green, yellow, white, oolong, black, Pu'er, and jasmine tea products, using high-resolution continuum source graphite furnace atomic absorption spectrometry. The methods used for sample preparation, digestion, and quantificational analysis were established, generating satisfactory analytical precisions (represented by relative standard deviations ranging from 0.6% to 2.5%) and recoveries (98.91-101.32%). The lead contents in tea leaves were 0.48-10.57 mg/kg, and 80% of these values were below the maximum values stated by the guidelines in China. The contents of cadmium and chromium ranged from 0.01 mg/kg to 0.39 mg/kg and from 0.27 mg/kg to 2.45 mg/kg, respectively, remaining in compliance with the limits stipulated by China's Ministry of Agriculture. The copper contents were 7.73-63.71 mg/kg; only 64% of these values complied with the standards stipulated by the Ministry of Agriculture. The nickel contents ranged from 2.70 mg/kg to 13.41 mg/kg. Consequently, more attention must be paid to the risks of heavy metal contamination in tea. The quantitative method established in this work lays a foundation for preventing heavy metal toxicity in human from drinking tea and will help establish regulations to control the contents of heavy metals in tea. Copyright © 2015. Published by Elsevier B.V.

  10. Comparison of two methods for blood lead analysis in cattle: graphite-furnace atomic absorption spectrometry and LeadCare(R) II system.

    Science.gov (United States)

    Bischoff, Karyn; Gaskill, Cynthia; Erb, Hollis N; Ebel, Joseph G; Hillebrandt, Joseph

    2010-09-01

    The current study compared the LeadCare(R) II test kit system with graphite-furnace atomic absorption spectrometry for blood lead (Pb) analysis in 56 cattle accidentally exposed to Pb in the field. Blood Pb concentrations were determined by LeadCare II within 4 hr of collection and after 72 hr of refrigeration. Blood Pb concentrations were determined by atomic absorption spectrometry, and samples that were coagulated (n = 12) were homogenized before analysis. There was strong rank correlation (R(2) = 0.96) between atomic absorption and LeadCare II (within 4 hr of collection), and a conversion formula was determined for values within the observed range (3-91 mcg/dl, although few had values >40 mcg/dl). Median and mean blood pb concentrations for atomic absorption were 7.7 and 15.9 mcg/dl, respectively; for LeadCare II, medians were 5.2 mcg/dl at 4 hr and 4.9 mcg/dl at 72 hr, and means were 12.4 and 11.7, respectively. LeadCare II results at 4 hr strongly correlated with 72 hr results (R(2) = 0.96), but results at 72 hr were lower (P atomic absorption. Although there have been several articles that compared LeadCare with other analytical techniques, all were for the original system, not LeadCare II. The present study indicated that LeadCare II results correlated well with atomic absorption over a wide range of blood Pb concentrations and that refrigerating samples for up to 72 hr before LeadCare II analysis was acceptable for clinical purposes.

  11. A sensitive magnetic nanoparticle-based immunoassay of phosphorylated acetylcholinesterase using protein cage templated lead phosphate for signal amplification with graphite furnace atomic absorption spectrometry detection.

    Science.gov (United States)

    Liang, Pei; Kang, Caiyan; Yang, Enjian; Ge, Xiaoxiao; Du, Dan; Lin, Yuehe

    2016-04-07

    We developed a new magnetic nanoparticle sandwich-like immunoassay using protein cage nanoparticles (PCN) for signal amplification together with graphite furnace atomic absorption spectrometry (GFAAS) for the quantification of an organophosphorylated acetylcholinesterase adduct (OP-AChE), the biomarker of exposure to organophosphate pesticides (OPs) and nerve agents. OP-AChE adducts were firstly captured by titanium dioxide coated magnetic nanoparticles (TiO2-MNPs) from the sample matrixes through metal chelation with phospho-moieties, and then selectively recognized by anti-AChE antibody labeled on PCN which was packed with lead phosphate in its cavity (PCN-anti-AChE). The sandwich-like immunoreaction was performed among TiO2-MNPs, OP-AChE and PCN-anti-AChE to form a TiO2-MNP/OP-AChE/PCN-anti-AChE immunocomplex. The complex could be easily isolated from the sample solution with the help of magnet, and the released lead ions from PCN were detected by GFAAS for the quantification of OP-AChE. Greatly enhanced sensitivity was achieved because PCN increased the amount of metal ions in the cavity of each apoferritin. The proposed immunoassay yielded a linear response over a broad range of OP-AChE concentrations from 0.01 nM to 2 nM, with a detection limit of 2 pM, which has enough sensitivity for monitoring of low-dose exposure to OPs. This new method showed an acceptable stability and reproducibility and was validated with OP-AChE spiked human plasma.

  12. Determination of Pb (Lead, Cd (Cadmium, Cr (Chromium, Cu (Copper, and Ni (Nickel in Chinese tea with high-resolution continuum source graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Wen-Si Zhong

    2016-01-01

    Full Text Available The contents of lead, cadmium, chromium, copper, and nickel were determined in 25 tea samples from China, including green, yellow, white, oolong, black, Pu'er, and jasmine tea products, using high-resolution continuum source graphite furnace atomic absorption spectrometry. The methods used for sample preparation, digestion, and quantificational analysis were established, generating satisfactory analytical precisions (represented by relative standard deviations ranging from 0.6% to 2.5% and recoveries (98.91–101.32%. The lead contents in tea leaves were 0.48–10.57 mg/kg, and 80% of these values were below the maximum values stated by the guidelines in China. The contents of cadmium and chromium ranged from 0.01 mg/kg to 0.39 mg/kg and from 0.27 mg/kg to 2.45 mg/kg, respectively, remaining in compliance with the limits stipulated by China's Ministry of Agriculture. The copper contents were 7.73–63.71 mg/kg; only 64% of these values complied with the standards stipulated by the Ministry of Agriculture. The nickel contents ranged from 2.70 mg/kg to 13.41 mg/kg. Consequently, more attention must be paid to the risks of heavy metal contamination in tea. The quantitative method established in this work lays a foundation for preventing heavy metal toxicity in human from drinking tea and will help establish regulations to control the contents of heavy metals in tea.

  13. Trace determination of lead, chromium and cadmium in herbal medicines using ultrasound-assisted emulsification microextraction combined with graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Aghamohammadi, Mohammad; Faraji, Mahya; Shahdousti, Parvin; Kalhor, Hamideh; Saleh, Abolfazl

    2015-01-01

    The World Health Organization (WHO) recommends that medicinal plants should be checked for the presence of heavy metals. A preconcentration and separation technique for trace amounts of heavy metals from plant matrix is necessary in order to increase the sensitivity and precision of their determination. Lead, chromium and cadmium contaminations in herbal medicines were monitored using ultrasound-assisted emulsification microextraction (USAEME) combined with graphite furnace atomic absorption spectrometry (GF-AAS). In this work, the metal ions in the aqueous solution were complexed with ammonium pyrrolidine dithiocarbamate (APDC) and were extracted into 45 μL of toluene that was sonically dispersed in the aqueous phase. The emulsion formed was centrifuged and 20 μL of separated toluene was injected into a GF-AAS for analysis. Several factors including the kind of extraction solvent and its volume, sample pH, ionic strength and concentration of APDC were optimised. The linear dynamic range (LDR) values were in the range of 0.05 to 20 µg/L and the limit of detection values were in the range of 0.002-0.03 µg/L for target heavy metals. Enrichment factors were obtained in the range of 70-500. The precision of the proposed method was ≤ 8% (n = 5). The obtained amounts of Pb, Cr and Cd in selected herbal medicines were in the standard range, according to the WHO reports. The USAEME with GF-AAS procedure was shown to be an efficient, rapid, inexpensive and eco-friendly method for the determination of lead, chromium and cadmium in herbal medicines. Application of the USAEME method leads to an increased extraction efficiency with satisfactory precision in a short time using an extraction solvent volume at the microlitre level. Copyright © 2015 John Wiley & Sons, Ltd.

  14. Study of the roles of chemical modifiers in determining boron using graphite furnace atomic absorption spectrometry and optimization of the temperature profile during atomization.

    Science.gov (United States)

    Yamamoto, Yuhei; Shirasaki, Toshihiro; Yonetani, Akira; Imai, Shoji

    2015-01-01

    The measurement conditions for determining boron using graphite furnace-atomic absorption spectrometry (GF-AAS) were investigated. Differences in the boron absorbance profiles were found using three different commercially available GF-AAS instruments when the graphite atomizers in them were not tuned. The boron absorbances found with and without adjusting the graphite atomizers suggested that achieving an adequate absorbance for the determination of boron requires a sharp temperature profile that overshoots the target temperature during the atomization process. Chemical modifiers that could improve the boron absorbance without the need for using coating agents were tested. Calcium carbonate improved the boron absorbance but did not suppress variability in the peak height. Improvement of boron absorbance was comparatively less using iron nitrate or copper nitrate than using calcium carbonate, but variability in the peak height was clearly suppressed using iron nitrate or copper nitrate. The limit of detection was 0.0026 mg L(-1) when iron nitrate was used. It appears that iron nitrate is a useful new chemical modifier for the quick and simple determination of boron using GF-AAS.

  15. Magnetic solid-phase extraction combined with graphite furnace atomic absorption spectrometry for speciation of Cr(III) and Cr(VI) in environmental waters.

    Science.gov (United States)

    Jiang, Hong-mei; Yang, Ting; Wang, Yan-hong; Lian, Hong-zhen; Hu, Xin

    2013-11-15

    A new approach of magnetic solid phase extraction (MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) has been developed for the speciation of Cr(III) and Cr(VI) using zincon-immobilized silica-coated magnetic Fe3O4 nanoparticles (Zincon-Si-MNPs) as the MSPE absorbent. Cr(III) was quantitatively reserved on the absorbent at pH 9.1 while total Cr was reserved at pH 6.5. The absorbed Cr species were eluted by using 2 mol/L HCl and detected by GFAAS. The concentration of Cr(VI) could be calculated by subtracting Cr(III) from total Cr. All the parameters affecting the separation and extraction efficiency of Cr species such as pH, extraction time, concentration and volume of eluent, sample volume and influence of co-existing ions were systematically examined and the optimized conditions were established accordingly. The detection limit (LOD) of the method was 0.016 and 0.011 ng mL(-1) for Cr(III) and Cr(VI), respectively, with the enrichment factor of 100 and 150. The precisions of this method (Relative standard deviation, RSD, n=7) for Cr(III) and Cr(VI) at 0.1 ng mL(-1) were 6.0% and 6.2%, respectively. In order to validate the proposed method, a certified reference material of environmental water was analyzed, and the result of Cr speciation was in good agreement with the certified value. This MSPE-GFAAS method has been successfully applied for the speciation of Cr(III) and Cr(VI) in lake and tap waters with the recoveries of 88-109% for the spiked samples. Moreover, the MSPE separation mechanism of Cr(III) and Cr(VI) based on their adsorption-desorption on Zincon-Si-MNPs has been explained through various spectroscopic characterization. © 2013 Elsevier B.V. All rights reserved.

  16. Application of Factorial Designs and Simplex Optimisation in the Development of Flow Injection-Hydride Generation-Graphite Furnace Atomic Absorption Spectrometry Procedures as Demonstrated for the Determination of Trace Levels of Germanium

    DEFF Research Database (Denmark)

    Hilligsøe, Bo; Hansen, Elo Harald

    1997-01-01

    The optimisation of a volume-based FI-HG-GFAAS procedure is described for the trace determination of Ge, comprising in situ collection of the generated germane in the graphite furnace. The response function is the peak area readout (A*s). Based on a preliminary study, where factorial designs were...

  17. Identification of molecules in graphite furnace by laser ionization time-of-flight mass spectrometry: sulfur and chlorine containing compounds

    CSIR Research Space (South Africa)

    Raseleka, RM

    2004-01-01

    Full Text Available An electro thermal vaporizer (ETV) coupled to a time-of-flight mass spectrometer (TOF-MS) with laser ionization (LI) was applied to the identification of molecules from sulphur and chlorine matrices in the furnace. An interface was developed...

  18. GUM Analysis for SIMS Isotopic Ratios in BEP0 Graphite Qualification Samples, Round 2

    Energy Technology Data Exchange (ETDEWEB)

    Gerlach, David C.; Heasler, Patrick G.; Reid, Bruce D.

    2009-01-01

    This report describes GUM calculations for TIMS and SIMS isotopic ratio measurements of reactor graphite samples. These isotopic ratios are used to estimate reactor burn-up, and currently consist of various ratios of U, Pu, and Boron impurities in the graphite samples. The GUM calculation is a propagation of error methodology that assigns uncertainties (in the form of standard error and confidence bound) to the final estimates.

  19. Development of a new green non-dispersive ionic liquid microextraction method in a narrow glass column for determination of cadmium prior to couple with graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa; Shah, Faheem; Afridi, Hassan Imran; Citak, Demirhan

    2014-02-17

    Easy and innovative non-dispersive ionic liquid based microextraction (NDILME) has been developed for preconcentration of trace level of cadmium (Cd) in aqueous real surface water samples prior to couple with graphite furnace atomic absorption spectrometry (GFAAS). A 200 cm long narrow glass column containing aqueous solution of standard/sample was used to increase phase transfer ratio by providing more contact area between two medium (aqueous and extractive), which drastically improve the recoveries of labile hydrophobic chelate of Cd ammonium pyrrolidinedithiocarbamate (APDC), into ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6]. Different aspect of the desire method have been investigated and optimized. Under the optimized key experimental variables, limit of detection (LOD) and enhancement factor (EF) were achieved to be 0.5 ng L(-1) and 150, respectively. Reliability of the model method was checked by relative standard deviation (%RSD), which was found to be water samples (SLRS-4 Riverine water) using standard addition method. Application of the model method was productively performed by analysis of Cd in real surface water samples (tap and sea). Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Graphite structure and magnetic parameters of flake graphite cast iron

    Science.gov (United States)

    Vértesy, G.; Uchimoto, T.; Takagi, T.; Tomáš, I.; Kage, H.

    2017-11-01

    Different matrix and graphite morphologies were generated by a special heat treatment in three chemically different series of flake graphite cast iron samples. As cast, furnace cooled and air cooled samples were investigated. The length of graphite particles and the pearlite volume of samples were determined by metallographic examination and these parameters were compared with the nondestructively measured magnetic parameters. Magnetic measurements were performed by the method of Magnetic Adaptive Testing, which is based on systematic measurement and evaluation of minor magnetic hysteresis loops. It was shown that linear correlation existed between the magnetic quantities and the graphite length, and also between the magnetic quantities and the relative pearlite content in the investigated cast iron. A numerical expression was also determined between magnetic descriptors and relative pearlite content, which does not depend on the detailed experimental conditions.

  1. A comparison of laser ablation-inductively coupled plasma-mass spectrometry and high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of bromine in polymers

    Science.gov (United States)

    de Gois, Jefferson S.; Van Malderen, Stijn J. M.; Cadorim, Heloisa R.; Welz, Bernhard; Vanhaecke, Frank

    2017-06-01

    This work describes the development and comparison of two methods for the direct determination of Br in polymer samples via solid sampling, one using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and the other using high-resolution continuum source graphite furnace molecular absorption spectrometry with direct solid sample analysis (HR-CS SS-GF MAS). The methods were optimized and their accuracy was evaluated by comparing the results obtained for 6 polymeric certified reference materials (CRMs) with the corresponding certified values. For Br determination with LA-ICP-MS, the 79Br+ signal could be monitored interference-free. For Br determination via HR-CS SS-GF MAS, the CaBr molecule was monitored at 625.315 nm with integration of the central pixel ± 1. Bromine quantification by LA-ICP-MS was performed via external calibration against a single CRM while using the 12C+ signal as an internal standard. With HR-CS SS-GF MAS, Br quantification could be accomplished using external calibration against aqueous standard solutions. Except for one LA-ICP-MS result, the concentrations obtained with both techniques were in agreement with the certified values within the experimental uncertainty as evidenced using a t-test (95% confidence level). The limit of quantification was determined to be 100 μg g- 1 Br for LA-ICP-MS and 10 μg g- 1 Br for HR-CS SS-GF MAS.

  2. Trace elements determination in high salinity petroleum produced formation water by high-resolution continuum source graphite furnace atomic absorption spectrometry after matrix separation using Chelex-100® resin

    Science.gov (United States)

    Freire, Aline Soares; Santelli, Ricardo Erthal

    2012-05-01

    This study describes a procedure used for the determination of trace metals (Co, Cu, Mn, Ni and Pb) in high salinity petroleum produced formation water (PFW) employing high-resolution continuum source graphite furnace atomic absorption spectrometry for detection and Chelex-100® resin for matrix elimination and analytes preconcentration. Using 15.0 mL of PFW for the separation/preconcentration, detection limits of 0.006, 0.07, 0.03, 0.08 and 0.02 μg L- 1 were obtained for Co, Cu, Mn, Ni and Pb, respectively. The accuracy of the proposed method was evaluated by analyzing three seawater certified reference materials and by recovery tests, and the data indicate that the methodology can be successfully applied to this kind of samples. The precision values, expressed as relative standard deviation (% RSD, n = 10) for 2.0 μg L- 1, were found to be 3.5, 4.0, 9.0, 5.3 and 5.9 for Co, Cu, Mn, Ni and Pb, respectively. The proposed procedure was applied for the determination of these metals in medium and high salinity PFW samples obtained from Brazilian offshore petroleum exploration platforms.

  3. Application of zinc sealed tube graphitization on sub-milligram samples using EnvironMICADAS

    Science.gov (United States)

    Rinyu, László; Orsovszki, Gergely; Futó, István; Veres, Mihály; Molnár, Mihály

    2015-10-01

    The aim of this study was to extend the utilization range of our sealed tube graphitization methods toward the microgram sample sizes on EnvironMICADAS accelerator mass spectrometer in the Institute for Nuclear Research of the Hungarian Academy of Sciences, Hertelendi Laboratory of Environmental Studies (ATOMKI HLES). To accomplish this purpose both methods, which are routinely used in ATOMKI HLES (TiH2-Zn-method and Zn-method) have been tested in the range of 25-250 μg carbon content. To exclude the side effects caused by the possible contamination by the chemical pretreatment and combustion of small samples, all micro-graphite targets have been produced by splitting CO2 gas from combusted samples containing 1 mg C and radiocarbon free fossil CO2 without any chemical preparation. The result of the comparison was that the Zn-method produces lower blank levels in the range of 25-100 μg carbon content than the combined TiH2-Zn method. For this reason, the Zn-method has been used for further optimization of the parameters of graphitization of samples with 25 μg carbon content. Based on the executed tests the optimal graphitization parameters for 25 μg carbon content are 2.5 mg iron catalyst, 2.5 mg zinc reagent and 450 °C graphitization temperature. With these parameters 3.1 ± 0.1 pMC average background level can be reached (based on measurement of 12 Zn-method target) and the available precision for modern samples was 0.9-1.0% using EnvironMICADAS.

  4. Laser-Excited Atomic Fluorescence and Ionization in a Graphite Furnace for the Determination of Metals and Nonmetals

    Science.gov (United States)

    Butcher, David James

    1990-01-01

    Here is reported novel instrumentation for atomic spectrometry that combined the use of a pulsed laser system as the light source and an electrothermal atomizer as the atom cell. The main goal of the research was to develop instrumentation that was more sensitive for elemental analysis than commercially available instruments and could be used to determine elements in real sample matrices. Laser excited atomic fluorescence spectrometry (LEAFS) in an electrothermal atomizer (ETA) was compared to ETA atomic absorption spectrometry (AAS) for the determination of thallium, manganese, and lead in food and agricultural standard reference materials (SRMs). Compared to ETA AAS, ETA LEAFS has a longer linear dynamic range (LDR) (5-7 orders of magnitude compared to 2-3 orders of magnitude) and higher sensitivity (10 ^{-16} to 10^{ -14} g as compared to 10^{ -13} to 10^{-11} g). Consequently, ETA LEAFS allows elemental analysis to be done over a wider range of concentrations with less dilution steps. Thallium was accurately determined in biological samples by ETA LEAFS at amounts five to one hundred times below the ETA AAS detection limit. ETA AAS and ETA LEAFS were compared for the determination of lead and manganese, and in general, the accuracies and precisions of ETA AAS were the same, with typical precisions between 3% and 6%. Fluorine was determined using laser excited molecular fluorescence spectrometry (LEMOFS) in an ETA. Molecular fluorescence from magnesium fluoride was collected, and the detection limit of 0.3 pg fluorine was two to six orders of magnitude more sensitive than other methods commonly used for the determination of fluorine. Significant interferences from ions were observed, but the sensitivity was high enough that fluorine could be determined in freeze dried urine SRMs by diluting the samples by a factor of one hundred to remove the interferences. Laser enhanced ionization (LEI) in an ETA was used for the determination of metals. For thallium, indium

  5. Determination of diphenylarsinic acid, phenylarsonic acid and inorganic arsenic in drinking water by graphite-furnace atomic-absorption spectrometry after simultaneous separation and preconcentration with solid-phase extraction disks.

    Science.gov (United States)

    Hagiwara, Kenta; Inui, Tetsuo; Koike, Yuya; Nakamura, Toshihiro

    2013-01-01

    A simple method of graphite-furnace atomic-absorption spectrometry (GFAAS) after solid-phase extraction (SPE) was developed for the determination of diphenylarsinic acid (DPAA), phenylarsonic acid (PAA), and inorganic arsenic (iAs) in drinking water. This method involves the simultaneous collection of DPAA, PAA, and iAs using three stacked SPE disks, i.e., an Empore SDB-XD disk (the upper layer), an activated carbon disk (the middle layer), and a Cation-SR disk loaded with Zr and Ca (ZrCa-CED; the lower layer). A 200-mL aqueous sample was adjusted to pH 3 with nitric acid and passed through the SPE disks at a flow rate of 15 mL min(-1), to concentrate DPAA on the SDB-XD disk, PAA on the activated carbon disk, and iAs on the ZrCa-CED. The As compounds were eluted from the disks with 10 mL of ethanol containing 0.5 mol L(-1) ammonia solution for DPAA, 20 mL of 1 mol L(-1) ammonia solution for PAA, and 20 mL of 6 mol L(-1) hydrochloric acid for iAs. The eluates of DPAA, PAA, and iAs were diluted to 20, 25, and 25 mL, respectively, with deionized water, and then analyzed by GFAAS. The detection limits of As (three-times the standard deviation (n = 3) of the blank values) were 0.13 and 0.16 μg L(-1) at enrichment factors of 10 and 8, respectively, using a 200-mL water sample. Spike tests with 2 μg (10 μg L(-1)) of DPAA, PAA, and iAs in 200 mL of tap water and bottled drinking water showed good recoveries (96.1-103.8%).

  6. Trace elements determination in high salinity petroleum produced formation water by high-resolution continuum source graphite furnace atomic absorption spectrometry after matrix separation using Chelex-100 Registered-Sign resin

    Energy Technology Data Exchange (ETDEWEB)

    Freire, Aline Soares [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Departamento de Quimica Analitica, Universidade Federal do Rio de Janeiro Av. Athos da Silveira Ramos 149, Centro de Tecnologia, Bloco A, Cidade Universitaria, Rio de Janeiro/RJ, 21941-909 (Brazil); Santelli, Ricardo Erthal, E-mail: santelli@iq.ufrj.br [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Departamento de Quimica Analitica, Universidade Federal do Rio de Janeiro Av. Athos da Silveira Ramos 149, Centro de Tecnologia, Bloco A, Cidade Universitaria, Rio de Janeiro/RJ, 21941-909 (Brazil)

    2012-05-15

    This study describes a procedure used for the determination of trace metals (Co, Cu, Mn, Ni and Pb) in high salinity petroleum produced formation water (PFW) employing high-resolution continuum source graphite furnace atomic absorption spectrometry for detection and Chelex-100 Registered-Sign resin for matrix elimination and analytes preconcentration. Using 15.0 mL of PFW for the separation/preconcentration, detection limits of 0.006, 0.07, 0.03, 0.08 and 0.02 {mu}g L{sup -1} were obtained for Co, Cu, Mn, Ni and Pb, respectively. The accuracy of the proposed method was evaluated by analyzing three seawater certified reference materials and by recovery tests, and the data indicate that the methodology can be successfully applied to this kind of samples. The precision values, expressed as relative standard deviation (% RSD, n = 10) for 2.0 {mu}g L{sup -1}, were found to be 3.5, 4.0, 9.0, 5.3 and 5.9 for Co, Cu, Mn, Ni and Pb, respectively. The proposed procedure was applied for the determination of these metals in medium and high salinity PFW samples obtained from Brazilian offshore petroleum exploration platforms. - Highlights: Black-Right-Pointing-Pointer Petroleum-produced formation water were analyzed for Co, Cu, Mn, Ni and Pb determination. Black-Right-Pointing-Pointer In batch analyte preconcentration/matrix separation using Chelex-100 Registered-Sign was used. Black-Right-Pointing-Pointer Detection limits between 0.006 and 0.08 {mu}g L{sup -1} were found by using HR-CS-GFAAS. Black-Right-Pointing-Pointer Trace elements characterization is possible using the developed method. Black-Right-Pointing-Pointer Maximum trace element concentrations found could support future Brazilian directives.

  7. Results of tuyere coke sampling with regard to application of appropriate coke strength after reaction (CSR) for a blast furnace

    OpenAIRE

    Shiau J-S.; Ko Y-C.; Ho C-K.; Hung M-T.

    2017-01-01

    Raising pulverized coal injection (PCI) will decrease coke rate, but increase the residence time of coke and abrasion in the blast furnace (BF). Thus, insufficient coke strength will generate more coke fines in the lower BF and result in lower permeability and production of hot metal (HM). For understanding the behavior of coke at various HM productivities, a tuyere coke sampler was used to collect the coke samples for measuring the coke strength. Firstly, ...

  8. A Comparison of Blood-lead Level (BLL) in Opium-dependant Addicts With Healthy Control Group Using the Graphite Furnace/atomic Absorption Spectroscopy (GF-AAS) Followed by Chemometric Analysis.

    Science.gov (United States)

    Amiri, Mojtaba; Amini, Ramin

    2012-08-01

    A comparison of oral/inhaled opium addicts with a healthy control group was investigated. Using the graphite furnace atomic absorption spectroscopy (GF-AAS) followed by chemometric analysis, sub-to-low µg L-1 concentrations of blood lead level (BLL) was detected in both the addict and the control groups. In this study, BLL of 78 subjects (Iranian volunteers) in two opium-addicted (patient group) and healthy control groups was evaluated. All the volunteers were men. The patient group was comprised of 39 patients who used opium orally or by inhalation with a mean age of 48.6 ± 7.3 years. The patient group was selected through systematic incidental sampling from 150 orally or by inhalation opium-addicted patients referred to Shariati Hospital located in Tehran .The control group (39 subjects) was matched with the patient group with regard to age and sex and with a mean age of 44.8 ± 5.6 years. The mean concentration of lead was found to be significantly lower (P = 0.0001) in control group (16.70 ± 12.51 μg/dL) compared to addicts (57.04 ± 46.03 μg/dL). When the addicts were divided into various age groups, there appeared to be a significant difference (p= 0.0451) in blood lead concentration as a function of age, however when the control group was considered, no difference was observed (P = 0.51). Also, a tendency (P = 0.048) towards increasing BLL with respect to BMI was observed due to drug consumption, but there was no significant variation between BLL concentration and BMI when the control group was considered (P = 0.35). It was observed that the BLL in opium-addicts was significantly higher than that of the healthy control group. The mean difference of both groups was statistically significant.

  9. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of arsenic and selenium in water and sediment by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Jones, Sandra R.; Garbarino, John R.

    1999-01-01

    Graphite furnace-atomic absorption spectrometry (GF-AAS) is a sensitive, precise, and accurate technique that can be used to determine arsenic and selenium in samples of water and sediment. The GF-AAS method has been developed to replace the hydride generation-atomic absorption spectrometry (HG-AAS) methods because the method detection limits are similar, bias and variability are comparable, and interferences are minimal. Advantages of the GF-AAS method include shorter sample preparation time, increased sample throughput from simultaneous multielement analysis, reduced amount of chemical waste, reduced sample volume requirements, increased linear concentration range, and the use of a more accurate digestion procedure. The linear concentration range for arsenic and selenium is 1 to 50 micrograms per liter in solution; the current method detection limit for arsenic in solution is 0.9 microgram per liter; the method detection limit for selenium in solution is 1 microgram per liter. This report describes results that were obtained using stop-flow and low-flow conditions during atomization. The bias and variability of the simultaneous determination of arsenic and selenium by GF-AAS under both conditions are supported with results from standard reference materials--water and sediment, real water samples, and spike recovery measurements. Arsenic and selenium results for all Standard Reference Water Samples analyzed were within one standard deviation of the most probable values. Long-term spike recoveries at 6.25, 25.0, 37.5 micrograms per liter in reagent-, ground-, and surface-water samples for arsenic averaged 103 plus or minus 2 percent using low-flow conditions and 104 plus or minus 4 percent using stop-flow conditions. Corresponding recoveries for selenium were 98 plus or minus 13 percent using low-flow conditions and 87 plus or minus 24 percent using stop-flow conditions. Spike recoveries at 25 micrograms per liter in 120 water samples ranged from 97 to 99 percent

  10. The degree of non-equilibrium microstructure of hardened steel samples taken during its melting in an electric arc furnace

    Directory of Open Access Journals (Sweden)

    Олександр Михайлович Скребцов

    2015-10-01

    Full Text Available Austenite to ferrite and pearlite transformation has not been studied enough for low-carbon peritectic steels. Experiments were carried out in the electric arc furnace. Samples of the liquid metal were taken during smelting; three sample at melting, oxidation and reduction as well as one sample from the bucket were taken. The optical binocular microscope Axio Imagez A2m (production of the German company Zeis AG was used to analyze the samples for the chemical composition of the elements and for the microstructure(ferrite and pearlite amount. It makes it possible to determine ferrite-to-pearlite relation in steel by means of the special program Thixomet Pro. Experimental percentage of ferrite was compared with the equilibrium percentage of ferrite calculated from the carbon content in the sample from the Fe-C phase diagram. It has been found that during charge melting experimental ferrite content is 0,52-1,7 equilibrium ferrite content. During the recovery period the microstructural heterogeneity stabilizes and is equal to 0,91-0,93 equilibrium heterogeneity. This ratio is in good agreement with the data available in literature. The amount of rejected finished metal as function of the temperature of the melt at the outlet of the furnace has been determined as well. The amount of rejected steel is minimum if steel is 1,052-1,07 times overheated above the liquidus point which is equal to the temperature of equilibrium microheterogeneity of the molten metal

  11. Separation and preconcentration of platinum-group metals from spent autocatalysts solutions using a hetero-polymeric S, N-containing sorbent and determination by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Eskina, Vasilina V; Dalnova, Olga A; Filatova, Daria G; Baranovskaya, Vasilisa B; Karpov, Yuri A

    2016-10-01

    This paper describes the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for determination of Pt, Pd and Rh after separation and concentration by original in-house developed heterochain polymer S, N-containing sorbent. The methods of sample preparation of spent ceramic-based autocatalysts were considered, two of which were used: autoclave decomposition in mixture of acids HCl:HNO3 (3:1) and high-temperature melting with K2S2O7. Both methods anyway limit the direct determination of analytes by HR CS GFAAS. Using the first method it is an incomplete digestion of spent autocatalysts samples, since the precipitate is Si, and the rhodium metal dissolves with difficulty and partially passes into solution. In contrast to the first method, the second method allow to completely transfer analytes into solution, however, the background signal produced by the chemical composition of the flux, overlaps the analytical zone. It was found, that Pt, Pd and Rh contained in the spent ceramic automotive catalysts could be effectively separated and concentrated by heterochain polymer S, N-containing sorbent, which has high sorption capacity, selectivity and resistant to dilute acids. The chosen HR CS GFAAS analysis conditions enable us to determine Pt, Pd and Rh with good metrological characteristics. The concentrations of Pt, Pd and Rh in two samples of automobile exhaust catalysts were found in range of 0.00015-0.00050; 0.170-0.189; 0.0180-0.0210wt%, respectively. The relative standard deviation obtained by HR CS GFAAS was not more than 5%. Limits of detection by HR CS GFAAS achieved were 6.2·10(-6)wt% for Pt, 1.8·10(-6)wt% for Pd, and 3.4·10(-6)wt% for Rh. Limits of determination achieved by HR CS GFAAS were 1.1·10(-5)wt% for Pt, 6.9·10(-5)wt% for Pd, and 8.3·10(-5)wt% for Rh. To control the accuracy of PGM in sorption concentrates by HR CS GFAAS method, it was appropriate to conduct an inter-method comparative experiment. The

  12. Arsenic speciation by hydride generation-quartz furnace atomic absorption spectrometry. Optimization of analytical parameters and application to environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Molenat, N.; Astruc, A.; Holeman, M.; Pinel, R. [Laboratoire de Chimie Analytique Bioinorganique et Environnement, Dept. de Chimie, Faculte des Sciences et Techniques, 64 - Pau (France); Maury, G. [Montpellier-2 Univ., 34 (France). Dept. de Chimie Organique Fine

    1999-11-01

    Analytical parameters of hydride generation, trapping, gas chromatography and atomic absorption spectrometry detection in a quartz cell furnace (HG/GC/QFAAS) device have been optimized in order to develop an efficient and sensitive method for arsenic compounds speciation. Good performances were obtained with absolute detection limits in the range of 0.1 - 0.5 ng for arsenite, arsenate, mono-methyl-arsonic acid (MMAA), dimethyl-arsinic acid (DMAA) and trimethyl-arsine oxide (TMAO). A pH selective reduction for inorganic arsenic speciation was successfully reported. Application to the accurate determination of arsenic compounds in different environmental samples was performed. (authors)

  13. Striking Graphite Bearing Clasts Found in Two Ordinary Chondrite Samples; NWA6169 and NWA8330

    Science.gov (United States)

    Johnson, Jessica M.; Zolensky, Michael E.; Chan, Queenie; Kring, David A.

    2015-01-01

    Meteorites play an integral role in understanding the history of the solar system. Not only can they contain some of the oldest material found in the solar system they also can contain material that is unique. Many lithologies are only found as foreign clasts within distinctly different host meteorites. In this investigation two foreign clasts within the meteorites, NWA6169 and NWA8330 were studied. The purpose of this investigation was to examine the mineralogy and petrography of the clasts within the samples. From there an identification and possible origin were to be inferred. NWA6169 is an unclassified ordinary chondrite that has a presumed petrologic type of L3. NWA8330 is a classified ordinary chondrite that has a petrologic type of LL3. Both meteorites were found to contain clasts that were similar; both modally were comprised of about 5% acicular graphite. Through SEM and Raman Spectroscopy it was found that they contained olivine, pyroxene, plagioclase, Fe-Ni sulfides, graphite, and metals. They were found to portray an igneous texture with relationships that suggest concurrent growth. Analytical microprobe results for NWA6169 revealed mineral compositions of Fa31-34, Fs23-83, and Ab7-85. For NWA8330 these were Fa28-32, Fs10-24, and Ab4-83. Only one similar material has been reported, in the L3 chondrite Krymka (Semenenko & Girich, 1995). The clast they described exhibited similar mineralogies including the unusual graphite. Krymka data displayed compositional values of Fa28.5-35.0 and Fs9-25.9. These ranges are fairly similar to that of NWA6169 and NWA8330. These samples may all be melt clasts, probably of impact origin. Two possibilities are (1) impact of a C-type asteroid onto the L chondrite parent asteroid, and (2) a piece of proto-earth ejected from the moon-forming collision event. These possibilities present abundant questions, and can be tested. The measurement of oxygen isotope compositions from the clasts should reveal the original source of the

  14. Results of tuyere coke sampling with regard to application of appropriate coke strength after reaction (CSR for a blast furnace

    Directory of Open Access Journals (Sweden)

    Shiau J-S.

    2017-01-01

    Full Text Available Raising pulverized coal injection (PCI will decrease coke rate, but increase the residence time of coke and abrasion in the blast furnace (BF. Thus, insufficient coke strength will generate more coke fines in the lower BF and result in lower permeability and production of hot metal (HM. For understanding the behavior of coke at various HM productivities, a tuyere coke sampler was used to collect the coke samples for measuring the coke strength. Firstly, the difference of sampled coke under the conditions of various HM productivities was explored. Secondly, the BF operating conditions and causes of generating more coke fines was correlated by testing the coke reaction rate after reaction. Finally, according to the above analysis results, the relative regression equations had been obtained for sampling coke properties, BF operation conditions and BF permeability. Furthermore, the coke strength after reaction (CSR quantitative target and its online system at various blast conditions were set to provide some reference for coke and HM production.

  15. Brazing graphite to graphite

    Science.gov (United States)

    Peterson, George R.

    1976-01-01

    Graphite is joined to graphite by employing both fine molybdenum powder as the brazing material and an annealing step that together produce a virtually metal-free joint exhibiting properties similar to those found in the parent graphite. Molybdenum powder is placed between the faying surfaces of two graphite parts and melted to form molybdenum carbide. The joint area is thereafter subjected to an annealing operation which diffuses the carbide away from the joint and into the graphite parts. Graphite dissolved by the dispersed molybdenum carbide precipitates into the joint area, replacing the molybdenum carbide to provide a joint of virtually graphite.

  16. Voltammetric determination of polyphenolic content as rosmarinic acid equivalent in tea samples using pencil graphite electrodes.

    Science.gov (United States)

    David, Iulia Gabriela; Buleandră, Mihaela; Popa, Dana Elena; Bîzgan, Ana-Maria Cristina; Moldovan, Zenovia; Badea, Irinel-Adriana; Iorgulescu, Emilia Elena; Tekiner, Tuğçe Ayça; Basaga, Huveyda

    2016-06-01

    The quasi-reversible, diffusion controlled behavior of rosmarinic acid (RA) on a disposable pencil graphite electrode (PGE) was established by cyclic voltammetry. Using the anodic oxidation peak presented by RA on the PGE a differential pulse voltammetric (DPV) method was developed for the quantitative determination of RA. The linear range was 10(-8) - 10(-5) M RA and the detection and quantification limits were 7.93 × 10(-9) M and 2.64 × 10(-8) M RA, respectively. The applicability of the developed method was tested by recovery studies and by the assessment of the total polyphenolic contents (TPCDPV) of green, white and black Turkish teas, which were found to be 40.74, 30.04 and 23.97 mg rosmarinic acid equivalent/g dry tea, respectively. These results were in good agreement with those obtained by the Folin-Ciocalteu method. The developed method is a sensitive and cheap tool for the rapid and precise evaluation of TPCDPV of tea samples.

  17. On plate graphite supported sample processing for simultaneous lipid and protein identification by matrix assisted laser desorption ionization mass spectrometry.

    Science.gov (United States)

    Calvano, Cosima Damiana; van der Werf, Inez Dorothé; Sabbatini, Luigia; Palmisano, Francesco

    2015-05-01

    The simultaneous identification of lipids and proteins by matrix assisted laser desorption ionization-mass spectrometry (MALDI-MS) after direct on-plate processing of micro-samples supported on colloidal graphite is demonstrated. Taking advantages of large surface area and thermal conductivity, graphite provided an ideal substrate for on-plate proteolysis and lipid extraction. Indeed proteins could be efficiently digested on-plate within 15 min, providing sequence coverages comparable to those obtained by conventional in-solution overnight digestion. Interestingly, detection of hydrophilic phosphorylated peptides could be easily achieved without any further enrichment step. Furthermore, lipids could be simultaneously extracted/identified without any additional treatment/processing step as demonstrated for model complex samples such as milk and egg. The present approach is simple, efficient, of large applicability and offers great promise for protein and lipid identification in very small samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Feasibility of high-resolution continuum source molecular absorption spectrometry in flame and furnace for sulphur determination in petroleum products

    Energy Technology Data Exchange (ETDEWEB)

    Kowalewska, Zofia, E-mail: zofia.kowalewska@obr.pl

    2011-07-15

    For the first time, high-resolution molecular absorption spectrometry with a high-intensity xenon lamp as radiation source has been applied for the determination of sulphur in crude oil and petroleum products. The samples were analysed as xylene solutions using vaporisation in acetylene-air flame or in an electrothermally heated graphite furnace. The sensitive rotational lines of the CS molecule, belonging to the {Delta}{nu} = 0 vibrational sequence within the electronic transition X{sup 1}{Sigma}{sup +} {yields} A{sup 1}{Pi}, were applied. For graphite furnace molecular absorption spectrometry, the Pd + Mg organic modifier was selected. Strong interactions with Pd atoms enable easier decomposition of sulphur-containing compounds, likely through the temporal formation of Pd{sub x}S{sub y} molecules. At the 258.056 nm line, with the wavelength range covering central pixel {+-} 5 pixels and with application of interactive background correction, the detection limit was 14 ng in graphite furnace molecular absorption spectrometry and 18 mg kg{sup -1} in flame molecular absorption spectrometry. Meanwhile, application of 2-points background correction found a characteristic mass of 12 ng in graphite furnace molecular absorption spectrometry and a characteristic concentration of 104 mg kg{sup -1} in flame molecular absorption spectrometry. The range of application of the proposed methods turned out to be significantly limited by the properties of the sulphur compounds of interest. In the case of volatile sulphur compounds, which can be present in light petroleum products, severe difficulties were encountered. On the contrary, heavy oils and residues from distillation as well as crude oil could be analysed using both flame and graphite furnace vaporisation. The good accuracy of the proposed methods for these samples was confirmed by their mutual consistency and the results from analysis of reference samples (certified reference materials and home reference materials with

  19. Fluid-deposited graphitic inclusions in quartz: Comparison between KTB (German Continental Deep-Drilling) core samples and artificially reequilibrated natural inclusions

    Science.gov (United States)

    Pasteris, J.D.; Chou, I.-Ming

    1998-01-01

    We used Raman microsampling spectroscopy (RMS) to determine the degree of crystallinity of minute (2-15 ??m) graphite inclusions in quartz in two sets of samples: experimentally reequilibrated fluid inclusions in a natural quartz grain and biotite-bearing paragneisses from the KTB deep drillhole in SE Germany. Our sequential reequilibration experiments at 725??C on initially pure CO2 inclusions in a quartz wafer and the J. Krautheim (1993) experiments at 900-1100??C on organic compounds heated in gold or platinum capsules suggest that, at a given temperature, (1) fluid-deposited graphite will have a lower crystallinity than metamorphosed organic matter and (2) that the crystallinity of fluid-deposited graphite is affected by the composition of the fluid from which it was deposited. We determined that the precipitation of more-crystalline graphite is favored by lower fH2 (higher fO2), and that the crystallinity of graphite is established by the conditions (including gas fugacities) that pertain as the fluid first reaches graphite saturation. Graphite inclusions within quartz grains in the KTB rocks show a wide range in crystallinity index, reflecting three episodes of carbon entrapment under different metamorphic conditions. Isolated graphite inclusions have the spectral properties of totally ordered, completely crystalline graphite. Such crystallinity suggests that the graphite was incorporated from the surrounding metasedimentary rocks, which underwent metamorphism at upper amphibolite-facies conditions. Much of the fluid-deposited graphite in fluid inclusions, however, shows some spectral disorder. The properties of that graphite resemble those of experimental precipitates at temperatures in excess of 700??C and at elevated pressures, suggesting that the inclusions represent precipitates from C-O-H fluids trapped under conditions near those of peak metamorphism at the KTB site. In contrast, graphite that is intimately associated with chlorite and other

  20. Stable Carbon Isotope Ratio (δ13C Measurement of Graphite Using EA-IRMS System

    Directory of Open Access Journals (Sweden)

    Andrius Garbaras

    2015-06-01

    Full Text Available δ13C values in non-irradiated natural graphite were measured. The measurements were carried out using an elemental analyzer combined with stable isotope ratio mass spectrometer (EA-IRMS. The samples were prepared with ground and non-ground graphite, the part of which was mixed with Mg (ClO42. The best combustion of graphite in the oxidation furnace of the elemental analyzer was achieved when the amount of pulverized graphite ranged from 200 to 490 µg and the mass ratio C:Mg(ClO42 was approximately 1:10. The method for the graphite burning avoiding the isotope fractionation is proposed.DOI: http://dx.doi.org/10.5755/j01.ms.21.2.6873

  1. Determination of Dissolved Iron in Seta River Water by Spectrophotometry using the Colored Complex of Ferrozine and Iron(II) and Graphite Furnace Atomic Absorption Spectrometry

    OpenAIRE

    原, 博一; 上野, 智子; 小林, 悠樹; 森山, さより; 西岡, 宏美

    2015-01-01

    The dissolved reactive iron(II) and iron(III) in the Seta River water were separately determinedby flow-injection spectrophotometry of the colored complex of ferrozine and iron(II). The reactiveiron(III) was determined after their reduction by a reducing agent, hydroxylamine hydrochloride.The sample volume needed for one determination was only 1mL and the determination can be donewithout any concentration procedure. The determination was done using two different buffersolutions of pH5.0 and 7...

  2. Electrostatic Levitation Furnace for the ISS

    Science.gov (United States)

    Murakami, Keiji; Koshikawa, Naokiyo; Shibasaki, Kohichi; Ishikawa, Takehiko; Okada, Junpei; Takada, Tetsuya; Arai, Tatsuya; Fujino, Naoki; Yamaura, Yukiko

    2012-01-01

    JAXA (Japan Aerospace Exploration Agency) has just started the development of Electrostatic Levitation Furnace to be launched in 2014 for the ISS. This furnace can control the sample position with electrostatic force and heat it above 2000 degree Celsius using semiconductor laser from four different directions. The announcement of Opportunity will be issued soon for this furnace. In this paper, we will show the specifications of this furnace and also the development schedule

  3. Trace Elements Analysis in Drinking Water of Meghalaya by Using Graphite Furnace-Atomic Absorption Spectroscopy and in relation to Environmental and Health Issues

    Directory of Open Access Journals (Sweden)

    Elarina N. Dkhar

    2014-01-01

    Full Text Available Determination of the certain major and trace elements was carried out in drinking water supply scheme in three districts of Meghalaya. This work aims to identify trends resulting in the deterioration of drinking water which is also a potential source of environmental contaminants. About 50 samples, each from one district, were collected both from the source and various tanks and tap. The elements determined are Li, Na, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Rb, Ag, Au, Pb, Cd, Se, Ca, K, and Mg. The pH is slightly lower than neutral pH of 7 while the turbidity is very high even after treatment. The concentrations of Ca and Mg are found to be deficient. The elements Cr, Fe, Co, Ni, Zn, Mo, and Pb decrease after treatment while Mn, Cu, and Cd increase slightly after treatment. Se concentration is found to be much higher than expected. The results were compared with the standard recommendation values for the quality of drinking water. This study provides a general indication of where water-quality constituent concentrations met or exceeded water-quality standards and the data presented in this report will be useful from public health point of view.

  4. Analysis of the bioavailability of Cr(III and Cr(VI based on the determination of chromium in Mentha piperita by graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    SVETLANA ĐOGO

    2011-01-01

    Full Text Available Mentha piperita L. (Lamiaceae was cultivated under the controlled laboratory conditions in the presence of varying levels of trivalent and hexavalent chromium in order to determine its capacity to control chromium uptake and its tolerance limit. The plants were grown in pots at 25 °C with controlled soil moisture (about 80 % of the water retention capacity. The soil was treated with increasing concentrations of Cr(NO33 (40, 80, 120, and 200 mg kg-1 and K2Cr2O7 (2.5, 5, 10, and 15 mg kg-1. A control group of plants was grown without the addition of chromium to the soil. For each concentration, three acidity levels were tested: natural, one pH unit below and one above the natural acidity of the soil (pH2 6, pH1 5 and pH3 7. The plant samples were digested according to the standard procedure and chromium content was determined by GFAAS. For all plants, the transportation index was calculated and the results (expressed in mg kg-1 at pH1, pH2 and pH3, respectively, were: 0.21–0.80, 0.06–1.06 and 0.04–0.52. The recoveries were good (72.73–115.3 % as evidenced by the analysis of certified reference materials (NIST SRM 8433 – Corn Bran and NIST SRM 1547 – Peach Leaves. The mobility of chromium through the plants tissues is discussed in regard to its competition with iron and manganese for transport binding sites; hence Mn and Fe were also determined.

  5. Flexible PVC flame retarded with expandable graphite

    CSIR Research Space (South Africa)

    Focke, WW

    2014-02-01

    Full Text Available furnace. Milled natural Zimbabwean flake graphite (Graphite) was supplied by BEP Bestobell (South Africa) and used as a reference material. TPC Paste Resin Co., Ltd. supplied the poly(vinyl chloride) emulsion grade PG680. It was a free flowing powder...

  6. short communication graphite furnace atomic absorption ...

    African Journals Online (AJOL)

    Preferred Customer

    2008-09-01

    2Department of Chemistry, Faculty of Sciences, Tarbiat-e-Moallem University of Sabzevar,. Sabzevar, Iran. (Received September 1, 2008; revised April 8, 2009). ABSTRACT. ABSTRACT. A method for the determination of trace amount of cadmium ion after preconcentration by extracting its dithizone complex into molten ...

  7. Graphite furnace atomic absorption spectrometric determination of ...

    African Journals Online (AJOL)

    A method for the determination of trace amount of cadmium ion after preconcentration by extracting its dithizone complex into molten naphthalene was developed. Several experimental conditions such as pH of the solution, stirring time, the amounts of naphthalene, standing time and volume of the solution were optimized.

  8. FIRE-RESISTANCE PROPERTIES RESEARCH OF “WATER GLASS - GRAPHITE MICROPARTICLES” COMPOSITE MATERIAL

    OpenAIRE

    E. A. Pitukhin; A. S. Ustinov

    2016-01-01

    Subject of Research. Research results of the fire-resistance for “water glass - graphite microparticles” composite material (CM) are given. The method for fire-resistance test of the micro composition is suggested in order to determine the limit state of the experimental samples under hightemperature action. Method. Test-benchequipment being used for research includes metering devices of temperature and time, as well as laboratory electric furnace PL20 with a maximum temperature in the chambe...

  9. Determination of cadmium and lead in perch fish samples by differential pulse anodic stripping voltammetry and furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Ahmed F. Al-Hossainy

    2017-02-01

    Full Text Available Lead and cadmium contents in the edible parts (muscle, fillet of 17 commercially used fish species from South Egypt River Nile (Aswan were determined by means of DPSAV (differential pulse stripping anodic voltammetry. In the sample preparation step, all fish samples were lyophilised, milled in a ball mill and finally decomposed by using mixed acid (HNO3 + HClO4. The accuracy of the concentrations determined in this study was checked by the measurements of the certified reference material CRM No. 422, cod muscle from the Commission of the European Communities, Community Bureau of Reference. All Pb2+ and Cd2+ concentrations observed from species of Egypt River Nile showed that fish from this area are a good source of these essential elements and the developed method is accepted as a good analytical routine method for these samples.

  10. Heat treatment furnace

    Energy Technology Data Exchange (ETDEWEB)

    Seals, Roland D; Parrott, Jeffrey G; DeMint, Paul D; Finney, Kevin R; Blue, Charles T

    2014-10-21

    A furnace heats through both infrared radiation and convective air utilizing an infrared/purge gas design that enables improved temperature control to enable more uniform treatment of workpieces. The furnace utilizes lamps, the electrical end connections of which are located in an enclosure outside the furnace chamber, with the lamps extending into the furnace chamber through openings in the wall of the chamber. The enclosure is purged with gas, which gas flows from the enclosure into the furnace chamber via the openings in the wall of the chamber so that the gas flows above and around the lamps and is heated to form a convective mechanism in heating parts.

  11. GRAPHITE EXTRUSIONS

    Science.gov (United States)

    Benziger, T.M.

    1959-01-20

    A new lubricant for graphite extrusion is described. In the past, graphite extrusion mixtures have bcen composed of coke or carbon black, together with a carbonaceous binder such as coal tar pitch, and a lubricant such as petrolatum or a colloidal suspension of graphite in glycerin or oil. Sinee sueh a lubricant is not soluble in, or compatible with the biiider liquid, such mixtures were difficult to extrude, and thc formed pieees lacked strength. This patent teaches tbe use of fatty acids as graphite extrusion lubricants and definite improvemcnts are realized thereby since the fatty acids are soluble in the binder liquid.

  12. Surface areas of turbostratic graphitic carbons prepared from a resin using nickel particles, 20 nm, as graphitization catalyst

    Energy Technology Data Exchange (ETDEWEB)

    Oya, A.; Inoue, E.; Otani, S.; Marsh, H.

    1981-11-01

    Nickel particles were used to graphitize catalytically a non-graphitizing carbon to create a turbostratic graphitic material called the T/SUB/s-component. This method was examined by X-ray diffraction. Coals on heat treatment to temperatures >1270 K form T/SUB/s-component carbons. Therefore, considerations of the properties of the T/SUB/s-component carbon may have relevance to considerations of the operational performances of blast furnace coke. (22 refs.)

  13. Analysis of Wigner energy release process in graphite stack of shut-down uranium-graphite reactor

    OpenAIRE

    Bespala, E. V.; Pavliuk, A. O.; Kotlyarevskiy, S. G.

    2015-01-01

    Data, which finding during thermal differential analysis of sampled irradiated graphite are presented. Results of computational modeling of Winger energy release process from irradiated graphite staking are demonstrated. It's shown, that spontaneous combustion of graphite possible only in adiabatic case.

  14. Effect of electropolishing on vacuum furnace design

    Directory of Open Access Journals (Sweden)

    Sutanwi Lahiri

    2015-03-01

    Full Text Available The use of thermal shields of materials having low emissivity in vacuum furnaces is well-known. However, the surface condition of the heat shields is one of the most important factors governing their efficiency as radiation resistances. The emissivity of the thermal shields dictates the power rating of the heaters in furnace design. The unpolished materials used in the heater tests showed poor performance leading to loss of a signi­ficant percentage of the input power. The present work deals with the refur­bishment of the radiation heat shields used in a furnace for heating graphite structure. The effect of refurbishment of the heat shields by the buffing and subsequently electro­polishing was found to improve the performance of the shields as heat reflectors. The com­position of the electrolyte was chosen in such a way that the large shields of Mo, Inconel and SS can be polished using the same reagents in different ratios. The present work deals with the development of a standard electropolishing procedure for large metallic sheets and subsequently qualifying them by roughness and emissivity measure­ments. The improvement noted in the shielding efficiency of the furnace in the subsequent runs is also discussed here.

  15. Cloud point extraction of iron(III) and vanadium(V) using 8-quinolinol derivatives and Triton X-100 and determination of 10(-7)moldm(-3) level iron(III) in riverine water reference by a graphite furnace atomic absorption spectroscopy.

    Science.gov (United States)

    Ohashi, Akira; Ito, Hiromi; Kanai, Chikako; Imura, Hisanori; Ohashi, Kousaburo

    2005-01-30

    The cloud point extraction behavior of iron(III) and vanadium(V) using 8-quinolinol derivatives (HA) such as 8-quinolinol (HQ), 2-methyl-8-quinolinol (HMQ), 5-butyloxymethyl-8-quinolinol (HO(4)Q), 5-hexyloxymethyl-8-quinolinol (HO(6)Q), and 2-methyl-5-octyloxymethyl-8-quinolinol (HMO(8)Q) and Triton X-100 solution was investigated. Iron(III) was extracted with HA and 4% (v/v) Triton X-100 in the pH range of 1.70-5.44. Above pH 4.0, more than 95% of iron(III) was extracted with HQ, HMQ, and HMO(8)Q. Vanadium(V) was also extracted with HA and 4% (v/v) Triton X-100 in the pH range of 2.07-5.00, and the extractability increased in the following order of HMQ extraction was applied to the determination of iron(III) in the riverine water reference by a graphite furnace atomic absorption spectroscopy. When 1.25 x 10(-3)M HMQ and 1% (v/v) Triton X-100 were used, the found values showed a good agreement with the certified ones within the 2% of the R.S.D. Moreover, the effect of an alkyl group on the solubility of 5-alkyloxymethyl-8-quinolinol and 2-methyl-5-alkyloxymethyl-8-quinolinol in 4% (v/v) Triton X-100 at 25 degrees C was also investigated.

  16. Raman characterization of bulk ferromagnetic nanostructured graphite

    Energy Technology Data Exchange (ETDEWEB)

    Pardo, Helena, E-mail: hpardo@fq.edu.uy [Centro NanoMat, Polo Tecnologico de Pando, Facultad de Quimica, Universidad de la Republica, Cno. Aparicio Saravia s/n, 91000, Pando, Canelones (Uruguay); Crystallography, Solid State and Materials Laboratory (Cryssmat-Lab), DETEMA, Facultad de Quimica, Universidad de la Republica, Gral. Flores 2124, P.O. Box 1157, Montevideo (Uruguay); Divine Khan, Ngwashi [Mantfort University, Leicester (United Kingdom); Faccio, Ricardo [Centro NanoMat, Polo Tecnologico de Pando, Facultad de Quimica, Universidad de la Republica, Cno. Aparicio Saravia s/n, 91000, Pando, Canelones (Uruguay); Crystallography, Solid State and Materials Laboratory (Cryssmat-Lab), DETEMA, Facultad de Quimica, Universidad de la Republica, Gral. Flores 2124, P.O. Box 1157, Montevideo (Uruguay); Araujo-Moreira, F.M. [Grupo de Materiais e Dispositivos-CMDMC, Departamento de Fisica e Engenharia Fisica, UFSCar, Caixa Postal 676, 13565-905, Sao Carlos SP (Brazil); Fernandez-Werner, Luciana [Centro NanoMat, Polo Tecnologico de Pando, Facultad de Quimica, Universidad de la Republica, Cno. Aparicio Saravia s/n, 91000, Pando, Canelones (Uruguay); Crystallography, Solid State and Materials Laboratory (Cryssmat-Lab), DETEMA, Facultad de Quimica, Universidad de la Republica, Gral. Flores 2124, P.O. Box 1157, Montevideo (Uruguay)

    2012-08-15

    Raman spectroscopy was used to characterize bulk ferromagnetic graphite samples prepared by controlled oxidation of commercial pristine graphite powder. The G:D band intensity ratio, the shape and position of the 2D band and the presence of a band around 2950 cm{sup -1} showed a high degree of disorder in the modified graphite sample, with a significant presence of exposed edges of graphitic planes as well as a high degree of attached hydrogen atoms.

  17. Effect of Carbon Aggregates on the Properties of Carbon Refractories for a Blast Furnace

    Science.gov (United States)

    Chen, Xilai; Li, Yawei; Li, Yuanbing; Sang, Shaobai; Zhao, Lei; Li, Shujing; Jin, Shengli; Ge, Shan

    2010-04-01

    The effect of carbon aggregates on the carbon refractory properties for a blast furnace was studied with X-ray diffraction (XRD), scanning electron microscopy (SEM), an energy-dispersive X-ray, mercury porosimetry, a resistivity instrument, and a laser thermal conductivity meter. The results showed that the microporous structure of a sample was determined by the amount of β-SiC whiskers. The thermal conductivity was controlled by the thermal conductivity of the corresponding carbon aggregate, and the alkali and molten-iron attack was decided mainly by the pore and the graphitization degree of aggregate, respectively. For samples using calcined anthracites as aggregates, the microporous structure became worse, the thermal conductivity increased, and the molten-iron as well as the alkali attack became more severe with an increase in the anthracite calcining temperature. For all samples, microcrystalline graphite possessed the best microporous structure and the least alkali and molten-iron attack, whereas the graphite electrode scraps had the highest thermal conductivity and the most severe alkali and molten-iron attack.

  18. Direct measurements of the thermal conductivity of various pyrolytic graphite samples (PG,TPG) used as thermal dissipation agents in detector applications

    CERN Document Server

    Heusch, C A; Kholodenko, A

    2002-01-01

    We performed model measurements on heat conduction in graphite-based structures, using several configurations. We describe our method for the direct measurement of thermal conductivity both in-plane and out-of-plane, for TPG and PG samples. Our results for the in-plane thermal conductivity coefficient, K sub a sub b were obtained with two different sets of boundary conditions; they are in good mutual agreement. Those for the transverse coefficient, K sub c , differ by a significant factor from the values published by the producers of the material.

  19. Vitrification of surrogate mixed wastes in a graphite electrode arc melter

    Energy Technology Data Exchange (ETDEWEB)

    Soelberg, N.R.; Chambers, A.G.; Ball, L. [and others

    1995-11-01

    Demonstration tests for vitrifying mixed wastes and contaminated soils have been conducted using a small (800 kVA), industrial-scale, three-phase AC, graphite electrode furnace located at the Albany Research Center of the United States Bureau of Mines (USBM). The feed mixtures were non-radioactive surrogates of various types of mixed (radioactive and hazardous), transuranic-contaminated wastes stored and buried at the Idaho National Engineering Laboratory (INEL). The feed mixtures were processed with added soil from the INEL. Objectives being evaluated include (1) equipment capability to achieve desired process conditions and vitrification products for different feed compositions, (2) slag and metals tapping capability, (3) partitioning of transuranic elements and toxic metals among the furnace products, (4) slag, fume, and metal products characteristics, and (5) performance of the feed, furnace and air pollution control systems. The tests were successfully completed in mid-April 1995. A very comprehensive process monitoring, sampling and analysis program was included in the test program. Sample analysis, data reduction, and results evaluation are currently underway. Initial results indicate that the furnace readily processed around 20,000 lb of widely ranging feed mixtures at feedrates of up to 1,100 lb/hr. Continuous feeding and slag tapping was achieved. Molten metal was also tapped twice during the test program. Offgas emissions were efficiently controlled as expected by a modified air pollution control system.

  20. New Experimental Technique for Nodularity and Mg Fading Control in Compacted Graphite Iron Production on Laboratory Scale

    Science.gov (United States)

    Hernando, Juan Carlos; Domeij, Björn; González, Daniel; Amieva, José Manuel; Diószegi, Attila

    2017-11-01

    The narrow production window for compacted graphite iron material (CGI) drastically reduces the possibilities to produce it in small batches outside an industrial environment. This fact hinders laboratory-scale investigations on CGI solidification. This work presents a solution to that issue by introducing an experimental technique to produce graphitic cast iron of the main three families. Samples of a base hypereutectic spheroidal graphite iron (SGI) were re-melted in a resistance furnace under Ar atmosphere. Varying the holding time at 1723 K (1450 °C), graphitic irons ranging from spheroidal to lamellar were produced. Characterization of the graphite morphology evolution, in terms of nodularity as a function of holding time, is presented. The nodularity decay for the SGI region suggests a linear correlation with the holding time. In the CGI region, nodularity deterioration shows a slower rate, concluding with the sudden appearance of lamellar graphite. The fading process of magnesium, showing agreement with previous researchers, is described by means of empirical relations as a function of holding time and nodularity. The results on nodularity fade and number of nodules per unit area fade suggest that both phenomena occur simultaneously during the fading process of magnesium.

  1. Calculations in furnace technology

    CERN Document Server

    Davies, Clive; Hopkins, DW; Owen, WS

    2013-01-01

    Calculations in Furnace Technology presents the theoretical and practical aspects of furnace technology. This book provides information pertinent to the development, application, and efficiency of furnace technology. Organized into eight chapters, this book begins with an overview of the exothermic reactions that occur when carbon, hydrogen, and sulfur are burned to release the energy available in the fuel. This text then evaluates the efficiencies to measure the quantity of fuel used, of flue gases leaving the plant, of air entering, and the heat lost to the surroundings. Other chapters consi

  2. Irradiation Creep in Graphite

    Energy Technology Data Exchange (ETDEWEB)

    Ubic, Rick; Butt, Darryl; Windes, William

    2014-03-13

    An understanding of the underlying mechanisms of irradiation creep in graphite material is required to correctly interpret experimental data, explain micromechanical modeling results, and predict whole-core behavior. This project will focus on experimental microscopic data to demonstrate the mechanism of irradiation creep. High-resolution transmission electron microscopy should be able to image both the dislocations in graphite and the irradiation-induced interstitial clusters that pin those dislocations. The team will first prepare and characterize nanoscale samples of virgin nuclear graphite in a transmission electron microscope. Additional samples will be irradiated to varying degrees at the Advanced Test Reactor (ATR) facility and similarly characterized. Researchers will record microstructures and crystal defects and suggest a mechanism for irradiation creep based on the results. In addition, the purchase of a tensile holder for a transmission electron microscope will allow, for the first time, in situ observation of creep behavior on the microstructure and crystallographic defects.

  3. Fast Determination of Iron and Zinc in Hair and Human Serum Samples After Alkaline Solubilization by GF AAS

    OpenAIRE

    Donnici, Cláudio L.; Souza, Carolina C.; Beinner, Mark A.; Silva, José Bento B. da

    2016-01-01

    Methods for the development and validation for determination of iron and zinc in human serum and hair samples by graphite furnace atomic absorption spectrometry (GF AAS) were performed. Solubilization was immediate by manual agitation in both samples with a 10 mL volume sample plus deionized water. Optimum pyrolysis and atomization temperatures were obtained by pyrolysis and atomization temperature curves in both matrices. For serum samples, the best temperatures were 1400 and 2500 °C (Fe) an...

  4. Quantum dots-multiwalled carbon nanotubes nanoconjugate-modified pencil graphite electrode for ultratrace analysis of hemoglobin in dilute human blood samples.

    Science.gov (United States)

    Prasad, Bhim Bali; Prasad, Amrita; Tiwari, Mahavir Prasad

    2013-05-15

    A novel molecularly imprinted polymer, selective for human hemoglobin, was immobilized on the surface of CdS quantum dots-multiwalled carbon nanotubes nanoconjugate-modified pencil graphite electrode. The fabricated sensor was found to be water-compatible and biologically benign, since the molecular imprinting was exclusively carried out in water, without any protein denaturation and electrode fouling. Notably, the pencil graphite electrode modified with merely a nanoconjugate matrix might involve the onset possibilities of electrode passivation and protein denaturation. However, a polymer coating onto the nanoconjugate obviated such obstacle while evaluating human hemoglobin in an aqueous environment (pH 4.2). The quantification of the hemoglobin in the dilute whole blood samples varied in the linear range 27.8-444.0 ng mL(-1); and the detection limit was obtained as 6.73 ng mL(-1) (S/N=3), without any cross-reactivity and false-positives. The proposed sensor can be used as a cost effective sensor for hemoglobin, in clinical settings. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Electrical properties of alkali-activated slag composite with combined graphite/CNT filler

    Science.gov (United States)

    Rovnaník, P.; Míková, M.; Kusák, I.

    2017-10-01

    Alkali-activated industrial by-products such as blast furnace slag are known to possess properties which are comparable to or even better than those observed for ordinary Portland cement. The combination of alkali-activated slag matrix with conductive filler introduces new functionalities which are commonly known for self-sensing or self-heating concrete. The present paper discusses the effect of the mixture of two different conductive fillers, graphite powder and carbon nanotubes (CNTs), on the electrical properties of alkali-activated slag mortars. Prepared samples were also tested for their mechanical properties and microstructure was investigated by means of mercury intrusion porosimetry and scanning electron microscopy. The percolation threshold for the resistance was reached for the mixture containing 0.1% CNTs and 8% graphite powder.

  6. HEAT RESISTANCE OF GRAPHITIZED STEEL

    Directory of Open Access Journals (Sweden)

    V. O. Savchenko

    2014-06-01

    Full Text Available Purpose. The investigation of temperature dependences of steels' mechanical properties and heat resistance under conditions of thermal cyclic loads. It's necessary to determine the mechanical properties and heat resistance indices of graphitized steels and cast iron VCh400 within the temperature range of 20…800°С. Methodology. Graphitized steels of the following chemical composition (mass %: 0.61…1.04C; 1.19…1.59%Si; 0.32…0.37%Mn; 0.12…0.17%Al; 0.008…0.014%S and 0.016…0.025%Р have been heat-treated according to the mode: heating up to 810°С – holding for 2 hours; cooling down to 680°С – holding for 2 hours with further cooling using the furnace in order to provide the ferrite-pearlite metallic base with graphite inclusions. In order to determine heat resistance indices (heat stresses index K and the material's resistance criterion at thermal cyclic load C the indices of graphitized steels' and cast irons' mechanical properties in the temperature range of 20…800°С have been investigated. Findings. It has been established that as a result of lower carbon content and smaller quantity of graphite inclusions, graphitized steel exceeds such indices of nodular cast iron VCh400 as: tensile strength and plasticity at room and high temperatures, and also heat resistance criteria K and C. This steel can be used to manufacture articles operating under conditions of thermal cyclic loads. Originality. Tensile strength and percent elongation of graphitized steels within the temperature range of 20…800°С have been determined. Calculations of heat resistance criteria to the heat stresses index K and the material's resistance criterion at thermal cyclic loads C within the temperature range 20…800°С in comparison with nodular cast iron of VCh400 grade have been carried out. Practical value. The expediency of using graphitized steel for manufacturing of articles operating under conditions of thermal cyclic loads has been shown.

  7. High temperature aircraft research furnace facilities

    Science.gov (United States)

    Smith, James E., Jr.; Cashon, John L.

    1992-01-01

    Focus is on the design, fabrication, and development of the High Temperature Aircraft Research Furnace Facilities (HTARFF). The HTARFF was developed to process electrically conductive materials with high melting points in a low gravity environment. The basic principle of operation is to accurately translate a high temperature arc-plasma gas front as it orbits around a cylindrical sample, thereby making it possible to precisely traverse the entire surface of a sample. The furnace utilizes the gas-tungsten-arc-welding (GTAW) process, also commonly referred to as Tungsten-Inert-Gas (TIG). The HTARFF was developed to further research efforts in the areas of directional solidification, float-zone processing, welding in a low-gravity environment, and segregation effects in metals. The furnace is intended for use aboard the NASA-JSC Reduced Gravity Program KC-135A Aircraft.

  8. Better VPS Fabrication of Crucibles and Furnace Cartridges

    Science.gov (United States)

    Holmes, Richard R.; Zimmerman, Frank R.; O'Dell, J. Scott; McKechnie, Timothy N.

    2003-01-01

    An experimental investigation has shown that by (1) vacuum plasma spraying (VPS) of suitable refractory metal alloys on graphite mandrels, and then (2) heat-treating the VPS alloy deposits under suitable conditions, it is possible to fabricate improved crucibles and furnace cartridges that could be used at maximum temperatures between 1,400 and 1,600 C and that could withstand chemical attack by the materials to be heated in the crucibles and cartridges. Taken by itself, the basic concept of fabricating furnace cartridges by VPS of refractory materials onto graphite mandrels is not new; taken by itself, the basic concept of heat treatment of VPS deposits for use as other than furnace cartridges is also not new; however, prior to this investigation, experimental crucibles and furnace cartridges fabricated by VPS had not been heat treated and had been found to be relatively weak and brittle. Accordingly, the investigation was directed toward determining whether certain combinations of (1) refractory alloy compositions, (2) VPS parameters, and (3) heat-treatment parameters could result in VPS-fabricated components with increased ductility.

  9. Advances in the graphitization protocol at the Radiocarbon Laboratory of the Universidade Federal Fluminense (LAC-UFF) in Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Macario, Kita D., E-mail: kitamacario@gmail.com [Departamento de Física, Instituto deFísica, Universidade Federal Fluminense, Campus da Praia Vermelha, Av. Gal. Milton Tavares de Souza s/n°, Niterói, RJ, 24210-346 (Brazil); Oliveira, Fabiana M. [Departamento de Física, Instituto deFísica, Universidade Federal Fluminense, Campus da Praia Vermelha, Av. Gal. Milton Tavares de Souza s/n°, Niterói, RJ, 24210-346 (Brazil); Carvalho, Carla [Departamento de Geoquímica, Instituto de Química, Universidade Federal Fluminense, Campus do Valonguinho, Outeiro São João Batista, s/n°, Niterói, RJ, 24020-150 (Brazil); Santos, Guaciara M.; Xu, Xiaomei [Department of Earth System Science, B321 Croul Hall, University of California Irvine, Irvine, CA, 92697-3100 (United States); Chanca, Ingrid S.; Alves, Eduardo Q.; Jou, Renata M.; Oliveira, Maria Isabela; Pereira, Bruna B.; Moreira, Vinicius; Muniz, Marcelo C.; Linares, Roberto; Gomes, Paulo Roberto Silveira; Meigikos dos Anjos, Roberto [Departamento de Física, Instituto deFísica, Universidade Federal Fluminense, Campus da Praia Vermelha, Av. Gal. Milton Tavares de Souza s/n°, Niterói, RJ, 24210-346 (Brazil); and others

    2015-10-15

    In this paper, we summarize the sample preparation methods currently used at the Radiocarbon Laboratory of the Universidade Federal Fluminense (LAC-UFF) in Brazil. We also report on a series of results with regards to the graphitization protocol. Tests with different temperatures and baking times were performed, and carbon stable isotope ratios of graphite were measured by an EA–IRMS (elemental analyzer coupled with an isotopic ratio mass spectrometer) to infer the completeness of the graphitization reaction. We monitored the muffle furnace temperature using an independent thermocouple and found a −60 °C offset, which may have caused the lower graphitization yields (detected from the large isotopic fractionation on several reference materials targets). At a temperature of 520 °C, the isotopic fractionation in the graphitization reaction was systematically lower (−5‰ in average) and the overall scattering was reduced. As long as isotopic fractionation corrections are made using the online stable isotopes ratios provided by the AMS system, the accuracy of the {sup 14}C results should be maintained.

  10. Thermally exfoliated graphite oxide

    Science.gov (United States)

    Prud'Homme, Robert K. (Inventor); Aksay, Ilhan A. (Inventor); Abdala, Ahmed (Inventor)

    2011-01-01

    A modified graphite oxide material contains a thermally exfoliated graphite oxide with a surface area of from about 300 sq m/g to 2600 sq m/g, wherein the thermally exfoliated graphite oxide displays no signature of the original graphite and/or graphite oxide, as determined by X-ray diffraction.

  11. FURNACES OF ROTARY HEATING

    Directory of Open Access Journals (Sweden)

    S. L. Ровин

    2004-01-01

    Full Text Available In the article there are analyzed the different ways of thermal treatment and melting of polydisperse materials and there are presented the developed by authors original coaxial-cylinder furnace settings, allowing to increase considerably the efficiency and productivity of technological process.  

  12. Dispersive cleanup of acetonitrile extracts of tea samples by mixed multiwalled carbon nanotubes, primary secondary amine, and graphitized carbon black sorbents.

    Science.gov (United States)

    Zhao, Pengyue; Wang, Lei; Jiang, Yaping; Zhang, Fengzu; Pan, Canping

    2012-04-25

    A method for analysis of 37 pesticide residues in tea samples was developed and validated and was based on reversed-dispersive solid-phase extraction (r-DSPE) cleanup in acetonitrile solution, followed by liquid chromatography-electrospray tandem mass spectrometry determination. Green tea, oolong tea, and puer tea were selected as matrixes and represent the majority of tea types. Acetonitrile was used as the extraction solvent, with sodium chloride and magnesium sulfate enhancing partitioning of analytes into the organic phase. The extract was then cleaned up by r-DSPE using a mixture of multiwalled carbon nanotubes, primary secondary amine, and graphitized carbon black as sorbents to absorb interferences. Further optimization of sample preparation and determination allowed recoveries of between 70% and 111% for all 37 pesticides with relative standard deviations lower than 14% at two concentration levels of 10 and 100 μg kg(-1). Limits of quantification ranged from 5 to 20 μg kg(-1) for all pesticides. The developed method was successfully applied to the determination of pesticide residues in market tea samples.

  13. Bridged graphite oxide materials

    Science.gov (United States)

    Herrera-Alonso, Margarita (Inventor); McAllister, Michael J. (Inventor); Aksay, Ilhan A. (Inventor); Prud'homme, Robert K. (Inventor)

    2010-01-01

    Bridged graphite oxide material comprising graphite sheets bridged by at least one diamine bridging group. The bridged graphite oxide material may be incorporated in polymer composites or used in adsorption media.

  14. A sensitive, selective and rapid determination of lead(II) ions in real-life samples using an electrochemically reduced graphene oxide-graphite reinforced carbon electrode.

    Science.gov (United States)

    Hamsawahini, Kunashegaran; Sathishkumar, Palanivel; Ahamad, Rahmalan; Yusoff, Abdull Rahim Mohd

    2015-11-01

    In this study, a sensitive and cost-effective electrochemically reduced graphene oxide (ErGO) on graphite reinforced carbon (GRC) was developed for the detection of lead (Pb(II)) ions present in the real-life samples. A film of graphene oxide (GO) was drop-casted on GRC and their electrochemical properties were investigated using cyclic voltammetry (CV), amperometry and square wave voltammetry (SWV). Factors influencing the detection of Pb(II) ions, such as grades of GRC, constant applied cathodic potential (CACP), concentration of hydrochloric acid and drop-casting drying time were optimised. GO is irreversibly reduced in the range of -0.7 V to -1.6 V vs Ag/AgCl (3 M) in acidic condition. The results showed that the reduction behaviour of GO contributed to the high sensitivity of Pb(II) ions detection even at nanomolar level. The ErGO-GRC showed the detection limit of 0.5 nM and linear range of 3-15 nM in HCl (1 M). The developed electrode has potential to be a good candidate for the determination of Pb(II) ions in different aqueous system. The proposed method gives a good recovery rate of Pb(II) ions in real-life water samples such as tap water and river water. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Carbothermal reduction process of silica formed from shirasu volcanic ash using solar furnace

    Directory of Open Access Journals (Sweden)

    Hatakeyama Keisuke

    2016-01-01

    Full Text Available Metallurgical grade silicon was formed using Shirasu volcanic ash as starting material with solar furnace. The solar furnace was composed of two parts: Fresnel lens and reacting furnace. The reacting furnace was composed of a cylindrical vacuum chamber and quartz glass plate functioning to guide the concentrated sunlight into the furnace, and was placed at the focal point of the Fresnel lens. The sample was made from a mixture of silica formed from Shirasu volcanic ash and carbon, and placed in the carbon crucible inside the reacting furnace. The sample was irradiated for 3 hours, and the furnace was left until it cooled down to room temperature. After the cooling process, the sample was mixed and placed in the carbon crucible, and it was irradiated and cooled with the same processes again. After the experiment, the sample was evaluated by X-ray diffraction and the production of silicon was confirmed.

  16. AGC-3 Graphite Preirradiation Data Analysis Report

    Energy Technology Data Exchange (ETDEWEB)

    William Windes; David Swank; David Rohrbaugh; Joseph Lord

    2013-09-01

    This report describes the specimen loading order and documents all pre-irradiation examination material property measurement data for the graphite specimens contained within the third Advanced Graphite Capsule (AGC-3) irradiation capsule. The AGC-3 capsule is third in six planned irradiation capsules comprising the Advanced Graphite Creep (AGC) test series. The AGC test series is used to irradiate graphite specimens allowing quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear graphite grades to be generated which will ascertain the in-service behavior of the graphite for pebble bed and prismatic Very High Temperature Reactor (VHTR) designs. The general design of AGC-3 test capsule is similar to the AGC-2 test capsule, material property tests were conducted on graphite specimens prior to loading into the AGC-3 irradiation assembly. However the 6 major nuclear graphite grades in AGC-2 were modified; two previous graphite grades (IG-430 and H-451) were eliminated and one was added (Mersen’s 2114 was added). Specimen testing from three graphite grades (PCEA, 2114, and NBG-17) was conducted at Idaho National Laboratory (INL) and specimen testing for two grades (IG-110 and NBG-18) were conducted at Oak Ridge National Laboratory (ORNL) from May 2011 to July 2013. This report also details the specimen loading methodology for the graphite specimens inside the AGC-3 irradiation capsule. The AGC-3 capsule design requires "matched pair" creep specimens that have similar dose levels above and below the neutron flux profile mid-plane to provide similar specimens with and without an applied load. This document utilized the neutron flux profile calculated for the AGC-3 capsule design, the capsule dimensions, and the size (length) of the selected graphite and silicon carbide samples to create a stacking order that can produce "matched pairs" of graphite samples above and below the AGC-3 capsule elevation mid-point to

  17. Fabrication of novel coated graphite electrodes for the selective nano-level determination of Cd{sup 2+} ions in biological and environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Jitendra [Department of Chemistry, Indian Institute of Technology-Roorkee, Roorkee 247 667 (India); Singh, Ashok Kumar, E-mail: akscyfcy@iitr.ernet.in [Department of Chemistry, Indian Institute of Technology-Roorkee, Roorkee 247 667 (India); Jain, A.K. [Department of Chemistry, Indian Institute of Technology-Roorkee, Roorkee 247 667 (India)

    2011-10-30

    Novel cadmium selective coated graphite electrodes were prepared using three different ionophores N{sup 1}, N{sup 2}-dicyanoethyl-N{sup 1}, N{sup 2}-bis(pyridin-2-ylmethyl)benzene-1, 2-diamine [L{sub 1}], N{sup 1}, N{sup 2}-dicyanoethyl-N{sup 1}, N{sup 2}-bis(thiophen-2-ylmethyl) benzene-1, 2-diamine [L{sub 2}] and N{sup 1}, N{sup 2}-dicyanoethyl-N{sup 1}, N{sup 2}-bis(furan-2-ylmethyl)benzene-1, 2-diamine [L{sub 3}], and their potentiometric characteristics were determined. Membranes having different compositions of poly(vinylchloride) (PVC), the plasticizer o-nitrophenyloctylether (o-NPOE), sodium tetraphenylborate (NaTPB) as an anionic additive and ionophores were coated onto the graphite surface. The potential response measurements showed that the best performance was exhibited by the electrodes with membranes having the composition L{sub 1}: o-NPOE:NaTPB:PVC as 4:51:2.5:42.5 (wt.%), L{sub 2}: o-NPOE:NaTPB:PVC as 3:52.5:1.5:43 (wt.%) and L{sub 3}: o-NPOE:NaTPB:PVC as 7:49:3.5:40.5 (wt.%). These electrodes had the widest working concentration range, Nernstian slope and fast response times of 12 s, 7 s and 17 s for L{sub 1}, L{sub 2} and L{sub 3}, respectively. The selectivity studies showed that these electrodes have higher selectivity towards Cd{sup 2+} over a large number of cations and could tolerate up to 20 vol.% non-aqueous impurities. Furthermore, the electrodes generated constant potentials in the pH range 2.0-8.0, with a shelf life of approximately four to six weeks. The high selectivity of these electrodes permits their use in the detection of the Cd{sup 2+} content in some medicinal plants, soil and industrial wastewater samples. The electrodes could also be used as an indicator electrode in the potentiometric titration of Cd{sup 2+} with EDTA.

  18. Development of multi-walled carbon nanotubes modified pencil graphite electrode for the electrochemical investigation of aceclofenac present in pharmaceutical and biological samples

    Directory of Open Access Journals (Sweden)

    P. Manjunatha

    2018-02-01

    Full Text Available A sensitive and novel chemically modified multi-walled carbon nanotubes modified pencil graphite electrode (MCPGE has been developed for the electrochemical investigation of aceclofenac (ACF. MCPGE was characterized by scanning electron microscopy (SEM, cyclic voltammetry (CV and electrochemical impedance spectroscopy (EIS. Phosphate buffer solution (PBS of pH 7.0 was used as a suitable electrolytic medium, in which aceclofenac (ACF exhibited a sensitive adsorption controlled oxidation peaks at +0.12, +0.32 and +0.51 V and a reduction peak at −0.26 V (vs Ag/AgCl. The experimental conditions were optimised by means of investigating the dependence of peak current on solution pH, concentration and scan rate etc. The electrochemical parameters such as surface concentration (Γ, electron transfer coefficient (α and the standard rate constant (ks were investigated at MCPGE. The oxidative peak currents were varied linearly with concentration in the range between 1 × 10−6 to 60 × 10−6 M with a detection limit of 2.6 × 10−9 M. The UV–Vis absorption spectrum of ACF gave the λmax at 272–273 nm and is attributed to the presence of ACF. The applicability of the MCPGE was illustrated by the determination of ACF present in pharmaceutical and human urine samples.

  19. Ultrasensitive photoelectrochemical determination of chromium(VI) in water samples by ion-imprinted/formate anion-incorporated graphitic carbon nitride nanostructured hybrid

    Energy Technology Data Exchange (ETDEWEB)

    Fang, Tian; Yang, Xiaomin; Zhang, Lizhi; Gong, Jingming, E-mail: jmgong@mail.ccnu.edu.cn

    2016-07-15

    Highlights: • IIP functionalized F-g-C{sub 3}N{sub 4} first applied to Cr(VI) detection. • The first smart integration of F-g-C{sub 3}N{sub 4} with IIP yielding a novel PEC sensing probe. • The system also explored for the speciation determination of chromium species. • The resulting sensor exhibiting fine applicability in real water samples. - Abstract: A rapid and highly sensitive photoelectrochemical (PEC) method has been proposed for the determination of trace amounts of chromium in water samples under visible-light irradiation. Here, a unique nanostructured hybrid of formate anion incorporated graphitic carbon nitride (F-g-C{sub 3}N{sub 4}) is smartly integrated with a Cr(VI) ion-imprinted polymer (IIP) as a photoactive electrode (denoted as IIP@F-g-C{sub 3}N{sub 4}). The nanohybrid of F-g-C{sub 3}N{sub 4} exhibits an enhanced charge separation with substantially improved PEC responses versus g-C{sub 3}N{sub 4}. The newly designed IIP@F-g-C{sub 3}N{sub 4} PEC sensor exhibits high sensitivity and selectivity for the determination of Cr(VI) because it offers efficient photogenerated electron reduction toward Cr(VI). The PEC analysis is highly linear over Cr(VI) concentrations ranging from 0.01 to 100.00 ppb with a detection limit of 0.006 ppb (S/N = 3). Our approach can be used to detect Cr(VI), Cr(III) and the total chromium level in aqueous solution through oxidation of Cr(III) to Cr(VI) and the determination of the total chromium as Cr(VI). In practical applications, this low-cost and sensitive assay has been successfully applied for speciation determination of chromium in environmental water samples.

  20. Arc ignition at heating of graphite by fixed current

    Science.gov (United States)

    Polistchook, V. P.; Samoylov, I. S.; Amirov, R. Kh; Kiselev, V. I.

    2017-11-01

    Arc ignition after the destruction of graphite samples under prolonged heating by electric current was described. Evidences of liquid film formation on the graphite surface at a temperature of 3.3 kK were presented.

  1. Properties and application of carbon composite brick for blast furnace hearth

    Directory of Open Access Journals (Sweden)

    Jiao K.X.

    2015-01-01

    Full Text Available A type of carbon composite brick was produced via the microporous technique using natural flack graphite, α-Al2O3 and high-quality bauxite chamotte (Al2O3≥87 mass% as raw materials with fine silicon powder as additive. The composition and microstructure of the obtained carbon composite were characterized using chemical analysis, XRD and SEM with EDS. The high temperature properties of thermal conductivity, oxidization and corrosion by molten slag and hot metal of the composite were analyzed. Based on these, the type of carbon composite brick worked in a blast furnace hearth for six years was further sampled at different positions. The protective layer was found and its chemical composition and microscopic morphology were investigated. It is found that the carbon composite brick combines the good properties of both the conventional carbon block and ceramic cup refractory. The protective layer near the hot face consists of two separated sublayers, i.e. the slag layer and the carbon layer. A certain amount of slag phase is contained in the carbon layer, which is caused by the reaction of coke ash with the refractory. No obvious change in the chemical composition of the protective layer along the depth of the sidewall is found. This work provides a useful guidance for the extension of the lifetime of blast furnace hearths.

  2. Improved Casting Furnace Conceptual Design

    Energy Technology Data Exchange (ETDEWEB)

    Fielding, Randall Sidney [Idaho National Lab. (INL), Idaho Falls, ID (United States); Tolman, David Donald [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2017-02-01

    In an attempt to ensure more consistent casting results and remove some schedule variance associated with casting, an improved casting furnace concept has been developed. The improved furnace uses the existing arc melter hardware and glovebox utilities. The furnace concept was designed around physical and operational requirements such as; a charge sized of less than 30 grams, high heating rates and minimal additional footprint. The conceptual model is shown in the report as well as a summary of how the requirements were met.

  3. Preparation of Ceramic-Bonded Carbon Block for Blast Furnace

    Science.gov (United States)

    Li, Yiwei; Li, Yawei; Sang, Shaobai; Chen, Xilai; Zhao, Lei; Li, Yuanbing; Li, Shujing

    2014-01-01

    Traditional carbon blocks for blast furnaces are mainly produced with electrically calcined anthracite owing to its good hot metal corrosion resistance. However, this kind of material shows low thermal conductivity and does not meet the demands for cooling of the hearth and the bottom of blast furnaces. In this article, a new kind of a high-performance carbon block has been prepared via ceramic-bonded carbon (CBC) technology in a coke bed at 1673 K (1400 °C) using artificial graphite aggregate, alumina, metallic aluminum, and silicon powders as starting materials. The results showed that artificial graphite aggregates were strongly bonded by the three-dimensional network of ceramic phases in carbon blocks. In this case, the good resistance of the CBC blocks against erosion/corrosion by the hot metal is provided by the ceramic matrix and the high thermal conductivity by the graphite aggregates. The microstructure of this carbon block resembles that of CBC composites with a mean pore size of less than 0.1 μm, and up to 90 pct of the porosity shows a pore size <1 μm. Its thermal conductivity is higher than 30 W · m-1 · K-1 [293 K (20 °C)]. Meanwhile, its hot metal corrosion resistance is better than that of traditional carbon blocks.

  4. Blast furnace hearth lining: post mortem analysis

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Bruno Vidal de; Vernilli Junior, Fernando, E-mail: bva@usp.br [Universidade de Sao Paulo (USP), Lorena, SP (Brazil). Escola de Engenharia; Neves; Elton Silva; Silva, Sidiney Nascimento [Companhia Siderugica Nacional (CSN), Rio de Janeiro, RJ (Brazil)

    2017-05-15

    The main refractory lining of blast furnace hearth is composed by carbon blocks that operates in continuous contact with hot gases, liquid slag and hot metal, in temperatures above 1550 deg C for 24 hours a day. To fully understand the wear mechanism that acts in this refractory layer system it was performed a Post Mortem study during the last partial repair of this furnace. The samples were collected from different parts of the hearth lining and characterized using the following techniques: Bulk Density and Apparent Porosity, X-Ray Fluorescence, X-ray Diffraction, Scanning Electron Microscopy with Energy-dispersive X-Ray Spectroscopy. The results showed that the carbon blocks located at the opposite side of the blast furnace tap hole kept its main physicochemical characteristics preserved even after the production of 20x10{sup 6} ton of hot metal. However, the carbon blocks around the Tap Hole showed infiltration by hot metal and slag and it presents a severe deposition of zinc and sulfur over its carbon flakes. The presence of these elements is undesired because it reduces the physic-chemical stability of this refractory system. This deposition found in the carbon refractory is associated with impurities present in the both coke and the sinter feed used in this blast furnace in the last few years. (author)

  5. In-situ pre-concentration through repeated sampling and pyrolysis for ultrasensitive determination of thallium in drinking water by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Liu, Liwei; Zheng, Huaili; Xu, Bincheng; Xiao, Lang; Chigan, Yong; Zhangluo, Yilan

    2018-03-01

    In this paper, a procedure for in-situ pre-concentration in graphite furnace by repeated sampling and pyrolysis is proposed for the determination of ultra-trace thallium in drinking water by graphite furnace atomic absorption spectrometry (GF-AAS). Without any other laborious enrichment processes that routinely result in analyte loss and contamination, thallium was directly concentrated in the graphite furnace automatically and subsequently subject to analysis. The effects of several key factors, such as the temperature for pyrolysis and atomization, the chemical modifier, and the repeated sampling times were investigated. Under the optimized conditions, a limit of detection of 0.01µgL -1 was obtained, which fulfilled thallium determination in drinking water by GB 5749-2006 regulated by China. Successful analysis of thallium in certified water samples and drinking water samples was demonstrated, with analytical results in good agreement with the certified values and those by inductively coupled plasma mass spectrometry (ICP-MS), respectively. Routine spike-recovery tests with randomly selected drinking water samples showed satisfactory results of 80-96%. The proposed method is simple and sensitive for screening of ultra-trace thallium in drinking water samples. Copyright © 2017. Published by Elsevier B.V.

  6. Metal-organic framework-199/graphite oxide hybrid composites coated solid-phase microextraction fibers coupled with gas chromatography for determination of organochlorine pesticides from complicated samples.

    Science.gov (United States)

    Zhang, Suling; Du, Zhuo; Li, Gongke

    2013-10-15

    The hybrid material of a copper-based metal-organic framework (MOF-199) and graphite oxide (GO) was explored as the solid-phase microextraction (SPME) coating for the first time. This fiber was fabricated by using 3-amino-propyltriethoxysilane (APTES) as the cross-linking agent, which enhanced its durability and allowed more than 140 replicate extractions. With the incorporation of GO, the MOF-199/GO fibers with GO contents ranging from 5 to 15 wt% exhibited enhanced adsorption affinity to organochlorine pesticides (OCPs) compared to MOF or GO individually. This improvement was linked to the enhanced dispersive forces (increased volume of small pores) that provided by the dense carbon layers of GO. Combining the superior properties of high porosity of MOFs and the unique layered character of GO, the MOF-199/GO (10 wt%) fiber exhibited higher adsorption affinity to some OCPs than commercial polydimethylsiloxane (PDMS) and polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibers. This new fiber was developed for headspace (HS) SPME of eight OCPs followed by GC/ECD analysis. The limits of detection were 2.3-6.9 ng/L. The relative standard deviation (RSD) for five replicate extractions using one fiber ranged from 5.3% to 8.8%. The fiber-to-fiber reproducibility was 5.2-12.8%. This method was successfully used for simultaneous determination of eight OCPs from river water, soil, water convolvulus and longan with satisfactory recoveries of 90.6-104.4%, 82.7-96.8%, 72.2-107.7% and 82.8-94.3%, respectively. These results indicated the MOF-199/GO composite provided a promising alternative in sample pretreatment. © 2013 Elsevier B.V. All rights reserved.

  7. Characterization of commercial expandable graphite fire retardants

    Energy Technology Data Exchange (ETDEWEB)

    Focke, Walter Wilhelm, E-mail: walter.focke@up.ac.za; Badenhorst, Heinrich; Mhike, Washington; Kruger, Hermanus Joachim; Lombaard, Dewan

    2014-05-01

    Highlights: • Expandable graphite is less well-ordered than its graphite bisulfate progenitor. • It includes graphite oxide as a randomly interstratified phase. • CO{sub 2}, CO and SO{sub 2} are released during thermal-driven exfoliation. - Abstract: Thermal analysis and other techniques were employed to characterize two expandable graphite samples. The expansion onset temperatures of the expandable graphite's were ca. 220 °C and 300 °C respectively. The key finding is that the commercial products are not just pure graphite intercalation compounds with sulfuric acid species intercalated as guest ions and molecules in between intact graphene layers. A more realistic model is proposed where graphite oxide-like layers are also randomly interstratified in the graphite flakes. These graphite oxide-like layers comprise highly oxidized graphene sheets which contain many different oxygen-containing functional groups. This model explains the high oxygen to sulfur atomic ratios found in both elemental analysis of the neat materials and in the gas generated during the main exfoliation event.

  8. STS Observations of Landau Levels at Graphite Surfaces

    OpenAIRE

    Matsui, T; Kambara, H.; Niimi, Y.; Tagami, K.; Tsukada, M.; Fukuyama, Hiroshi

    2004-01-01

    Scanning tunneling spectroscopy measurements were made on surfaces of two different kinds of graphite samples, Kish graphite and highly oriented pyrolytic graphite (HOPG), at very low temperatures and in high magnetic fields. We observed a series of peaks in the tunnel spectra, which grow with increasing field, both at positive and negative bias voltages. These are associated with Landau quantization of the quasi two-dimensional electrons and holes in graphite in magnetic fields perpendicular...

  9. Graphite Technology Development Plan

    Energy Technology Data Exchange (ETDEWEB)

    W. Windes; T. Burchell; M.Carroll

    2010-10-01

    The Next Generation Nuclear Plant (NGNP) will be a helium-cooled High Temperature Gas Reactor (HTGR) with a large graphite core. Graphite physically contains the fuel and comprises the majority of the core volume. Graphite has been used effectively as a structural and moderator material in both research and commercial high-temperature gas-cooled reactors. This development has resulted in graphite being established as a viable structural material for HTGRs. While the general characteristics necessary for producing nuclear grade graphite are understood, historical “nuclear” grades no longer exist. New grades must be fabricated, characterized, and irradiated to demonstrate that current grades of graphite exhibit acceptable non-irradiated and irradiated properties upon which the thermomechanical design of the structural graphite in NGNP is based. This Technology Development Plan outlines the research and development (R&D) activities and associated rationale necessary to qualify nuclear grade graphite for use within the NGNP reactor.

  10. Laser excited analytical atomic and ionic fluorescence in flames, furnaces and inductively coupled plasmas—I. General considerations

    Science.gov (United States)

    Omenetto, N.; Human, H. G. C.

    Several important parameters for the analytical use of laser excited fluorescence spectrometry in flames, graphite furnaces and inductively coupled plasmas are discussed in some detail. These parameters include the laser characteristics such as peak power, pulse duration, spectral bandwidth and repetition rate, the choice of the excitation line, the optical arrangement and the detection system, this last one centred on the widespread use of the boxcar averager. It is shown that, if the ultimate sensitivity is the goal to be achieved, then the choice must be the electrothermal atomization. However, even for flames and inductively coupled plasmas, excellent results are possible provided that: (i) the laser system allows complete spectral coverage in the ultraviolet: (ii) saturation of the fluorescence signal can be approached over a large sample volume; and (iii) the gated detection parameters and the laser repetition frequency are optimized with respect to each other so as to reach the maximum signal-to-noise ratio.

  11. Determination of indium in geological materials by electrothermal-atomization atomic absorption spectrometry with a tungsten-impregnated graphite furance

    Science.gov (United States)

    Zhou, L.; Chao, T.T.; Meier, A.L.

    1984-01-01

    The sample is fused with lithium metaborate and the melt is dissolved in 15% (v/v) hydrobromic acid. Iron(III) is reduced with ascorbic acid to avoid its coextraction with indium as the bromide into methyl isobutyl ketone. Impregnation of the graphite furnace with sodium tungstate, and the presence of lithium metaborate and ascorbic acid in the reaction medium improve the sensitivity and precision. The limits of determination are 0.025-16 mg kg-1 indium in the sample. For 22 geological reference samples containing more than 0.1 mg kg-1 indium, relative standard deviations ranged from 3.0 to 8.5% (average 5.7%). Recoveries of indium added to various samples ranged from 96.7 to 105.6% (average 100.2%). ?? 1984.

  12. Development of reactor graphite

    Science.gov (United States)

    Haag, G.; Mindermann, D.; Wilhelmi, G.; Persicke, H.; Ulsamer, W.

    1990-04-01

    The German graphite development programme for High Temperature Reactors has been based on the assumption that reactor graphite for core components with lifetime fluences of up to 4 × 10 22 neutrons per cm 2 (EDN) at 400°C can be manufactured from regular pitch coke. The use of secondary coke and vibrational moulding techniques have allowed production of materials with very small anisotropy, high strength, and high purity which are the most important properties of reactor graphite. A variety of graphite grades has been tested in fast neutron irradiation experiments. The results show that suitable graphites for modern High Temperature Reactors with spherical fuel elements are available.

  13. Furnace brazing under partial vacuum

    Science.gov (United States)

    Mckown, R. D.

    1979-01-01

    Brazing furnace utilizing partial-vacuum technique reduces tooling requirements and produces better bond. Benefit in that partial vacuum helps to dissociate metal oxides that inhibit metal flow and eliminates heavy tooling required to hold parts together during brazing.

  14. Review of furnace modeling

    Energy Technology Data Exchange (ETDEWEB)

    Krishna, C. R.

    1978-06-01

    There has been a spurt of recent activity in developing and applying numerical modeling to combustors and furnaces. The purpose of this review is to provide a brief overview of these recent developments and draw conclusions on the scope for further work in the area of modeling. A brief qualitative review of the various models that have been developed is presented. The models show a progressive recognition of the complexity of turbulence-chemistry interactions and attempts to include more recent submodels of such interactions. There are attempts to incorporate the three-dimensional character of fluid flows and solve the elliptic equations arising in recirculating flows. Flux models of radiation transfer are being included in the energy transport equations. Efficient numerical algorithms are being developd to solve the finite difference form of a set of elliptic, partial differential equations. The test of the success of modeling lies, obviously, in comparison with experimental measurements. Such experiments are being undertaken, but, the techniques of measurements also need development before detailed comparison can be made. The measurements made seem to indicate qualitative agreement of model predictions with limited laboratory measurements. It is concluded from the review that there is still need for development in several areas including turbulence (and turbulence-chemistry interactions) modeling, liquid and solid fuel introduction, interaction with the flow and combustion, models for soot formation, and experimental validation.

  15. Fossil fuel furnace reactor

    Science.gov (United States)

    Parkinson, William J.

    1987-01-01

    A fossil fuel furnace reactor is provided for simulating a continuous processing plant with a batch reactor. An internal reaction vessel contains a batch of shale oil, with the vessel having a relatively thin wall thickness for a heat transfer rate effective to simulate a process temperature history in the selected continuous processing plant. A heater jacket is disposed about the reactor vessel and defines a number of independent controllable temperature zones axially spaced along the reaction vessel. Each temperature zone can be energized to simulate a time-temperature history of process material through the continuous plant. A pressure vessel contains both the heater jacket and the reaction vessel at an operating pressure functionally selected to simulate the continuous processing plant. The process yield from the oil shale may be used as feedback information to software simulating operation of the continuous plant to provide operating parameters, i.e., temperature profiles, ambient atmosphere, operating pressure, material feed rates, etc., for simulation in the batch reactor.

  16. Síntese de nanotubos de carbono de parede simples por sublimação de grafite em atmosfera de hélio Synthesis of single-wall nanotubes by pyrolysis of graphite in helium atmosphere

    Directory of Open Access Journals (Sweden)

    José Gino Venegas Romero

    2002-02-01

    Full Text Available Macroscopic samples of fullerene nanostructures are obtained in a modified arc furnace using the electric arc method with a Helium atmosphere at low pressures. High purity graphite rods are used as electrodes but, when drilled and the orifices filled with powders of transition metals (Fe, Co, Ni acting as catalysts, the resulting particles are carbon nanostructures of the fullerene family, known as Single Wall Nanotubes (SWNTs. They have typical diameters of 1.4 nm, lengths up to tenths of microns and they are arranged together in bundles containing several SWNTs. Those samples are observed and analyzed using Scanning Electron Microscopy (SEM and Transmission Electron Microscopy (TEM techniques.

  17. AGC-2 Graphite Preirradiation Data Analysis Report

    Energy Technology Data Exchange (ETDEWEB)

    William Windes; W. David Swank; David Rohrbaugh; Joseph Lord

    2013-08-01

    This report described the specimen loading order and documents all pre-irradiation examination material property measurement data for the graphite specimens contained within the second Advanced Graphite Capsule (AGC-2) irradiation capsule. The AGC-2 capsule is the second in six planned irradiation capsules comprising the Advanced Graphite Creep (AGC) test series. The AGC test series is used to irradiate graphite specimens allowing quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear graphite grades to be generated which will ascertain the in-service behavior of the graphite for pebble bed and prismatic Very High Temperature Reactor (VHTR) designs. Similar to the AGC-1 specimen pre-irradiation examination report, material property tests were conducted on specimens from 18 nuclear graphite types but on an increased number of specimens (512) prior to loading into the AGC-2 irradiation assembly. All AGC-2 specimen testing was conducted at Idaho National Laboratory (INL) from October 2009 to August 2010. This report also details the specimen loading methodology for the graphite specimens inside the AGC-2 irradiation capsule. The AGC-2 capsule design requires “matched pair” creep specimens that have similar dose levels above and below the neutron flux profile mid-plane to provide similar specimens with and without an applied load. This document utilized the neutron flux profile calculated for the AGC-2 capsule design, the capsule dimensions, and the size (length) of the selected graphite and silicon carbide samples to create a stacking order that can produce “matched pairs” of graphite samples above and below the AGC-2 capsule elevation mid-point to provide specimens with similar neutron dose levels.

  18. Improved Blackbody Temperature Sensors for a Vacuum Furnace

    Science.gov (United States)

    Farmer, Jeff; Coppens, Chris; O'Dell, J. Scott; McKechnie, Timothy N.; Schofield, Elizabeth

    2009-01-01

    Some improvements have been made in the design and fabrication of blackbody sensors (BBSs) used to measure the temperature of a heater core in a vacuum furnace. Each BBS consists of a ring of thermally conductive, high-melting-temperature material with two tantalum-sheathed thermocouples attached at diametrically opposite points. The name "blackbody sensor" reflects the basic principle of operation. Heat is transferred between the ring and the furnace heater core primarily by blackbody radiation, heat is conducted through the ring to the thermocouples, and the temperature of the ring (and, hence, the temperature of the heater core) is measured by use of the thermocouples. Two main requirements have guided the development of these BBSs: (1) The rings should have as high an emissivity as possible in order to maximize the heat-transfer rate and thereby maximize temperature-monitoring performance and (2) the thermocouples must be joined to the rings in such a way as to ensure long-term, reliable intimate thermal contact. The problem of fabricating a BBS to satisfy these requirements is complicated by an application-specific prohibition against overheating and thereby damaging nearby instrumentation leads through the use of conventional furnace brazing or any other technique that involves heating the entire BBS and its surroundings. The problem is further complicated by another application-specific prohibition against damaging the thin tantalum thermocouple sheaths through the use of conventional welding to join the thermocouples to the ring. The first BBS rings were made of graphite. The tantalum-sheathed thermocouples were attached to the graphite rings by use of high-temperature graphite cements. The ring/thermocouple bonds thus formed were found to be weak and unreliable, and so graphite rings and graphite cements were abandoned. Now, each BBS ring is made from one of two materials: either tantalum or a molybdenum/titanium/zirconium alloy. The tantalum

  19. Reduction of calcium sulfate in a coal-fired circulating fluidized bed furnace

    Energy Technology Data Exchange (ETDEWEB)

    Talukdar, J.; Basu, P.; Greenblatt, J.H. [Technical University of Nova Scotia, Halifax, NS (Canada). Mechanical Engineering Dept.

    1996-07-01

    The overall utilisation of limestone for sulphur capture in a CFB combustor depends on the reactivity of the various calcium species in the bed. To study the re-emission of SO{sub 2} the reactivity of partially sulfated CaO was studied. The material used was bottom ash drained from a 165 MWe commercial CFB boiler furnace. The tests were performed in an electrically heated furnace. Reactivity rate constants were determined from the experimental results. The release of SO{sub 2} from CaSO{sub 4} increases with temperature as well as with the concentration of the reducing agents CO, char and graphite. Of the reducing agents considered, CO is most reactive, followed by char and then graphite. 12 refs., 17 figs., 5 tabs.

  20. Modeling of graphite oxide

    OpenAIRE

    Boukhvalov, D. W.; Katsnelson, M. I.

    2008-01-01

    Based on density functional calculations, optimized structures of graphite oxide are found for various coverage by oxygen and hydroxyl groups, as well as their ratio corresponding to the minimum of total energy. The model proposed describes well known experimental results. In particular, it explains why it is so difficult to reduce the graphite oxide up to pure graphene. Evolution of the electronic structure of graphite oxide with the coverage change is investigated.

  1. A graphite nanoeraser

    DEFF Research Database (Denmark)

    Liu, Ze; Bøggild, Peter; Yang, Jia-rui

    2011-01-01

    We present here a method for cleaning intermediate-size (up to 50 nm) contamination from highly oriented pyrolytic graphite and graphene. Electron-beam-induced deposition of carbonaceous material on graphene and graphite surfaces inside a scanning electron microscope, which is difficult to remove...... by conventional techniques, can be removed by direct mechanical wiping using a graphite nanoeraser, thus drastically reducing the amount of contamination. We discuss potential applications of this cleaning procedure....

  2. Internal features of graphite in cast irons. Confocal microscopy: useful tool for graphite growth imaging.

    Science.gov (United States)

    Llorca-Isern, N; Tartera, J; Espanol, M; Marsal, M; Bertran, G; Castel, S

    2002-01-01

    Spherulitic crystallisation is a mode of growth of crystals from the melt. Considerable attention has been given to spheroidal graphite formation, providing detailed information about the internal microstructure of the spherulites in spheroidal (SG irons) and compacted graphite irons (CG irons) (Stefanescu, D., 1990. Cast Irons. ASM Handbook, 10th ed., vol. 1). Nevertheless, the mechanisms responsible for this mode of crystallisation are not fully understood. This study deals with the inoculation mechanisms, with particular emphasis on the study of the inclusions for the heterogeneous nucleation of graphite. It is shown that the graphite nuclei are sulfide products of the nodularizing treatment. It has been observed that when rare-earth treatment is applied, the central nucleus consists of a core and an envelope from which the graphite grows. Confocal Scanning Laser Microscopy (CSLM), in reflection mode, was used to study the internal features of the spheroidal graphite growth. Confocal reflection imaging, which has a capacity for optical sectioning of the sample, provides high-resolution images of surface and subsurface regions of interest contained within a semi-transparent sample. Furthermore, three-dimensional reconstruction of these optical sections can provide insight into the mechanism of graphite growth mechanism interpretation. With CSLM the radial growth of graphite was seen. Other techniques, such as TEM, SEM-EDS, WDS, AES and SAM were also used to corroborate the results.

  3. Advances in chemical and physical properties of electric arc furnace carbon steel slag by hot stage processing and mineral mixing

    Energy Technology Data Exchange (ETDEWEB)

    Liapis, Ioannis, E-mail: iliapis@sidenor.vionet.gr [AEIFOROS SA, 12th km Thessaloniki-Veroia Rd, PO Box 59, 57008 Ionia, Thessaloniki (Greece); Papayianni, Ioanna [Laboratory of Building Materials, Department of Civil Engineering, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece)

    2015-02-11

    Highlights: • Addition of 10% perlite decreases specific weight of the slag by approx. 7.5%. • Slag-crucible interaction and thin coating layer result in variations in XRF. • XRD shows high glass content and smaller crystalline sizes due to rapid cooling. • SEM shows higher homogeneity and lower crystallisation for SiO{sub 2}/CaO-rich samples. • Physical properties (LA, PSV, AAV) of modified slag show limited deterioration. - Abstract: Slags are recognised as a highly efficient, cost effective tool in the metal processing industry, by minimising heat losses, reducing metal oxidation through contact with air, removing metal impurities and protecting refractories and graphite electrodes. When compared to natural aggregates for use in the construction industry, slags have higher specific weight that acts as an economic deterrent. A method of altering the specific weight of EAFC slag by hot stage processing and mineral mixing, during steel production is presented in this article. The method has minimal interference with the production process of steel, even by limited additions of appropriate minerals at high temperatures. Five minerals are examined, namely perlite, ladle furnace slag, bauxite, diatomite and olivine. Measurements of specific weight are accompanied by X-ray diffraction (XRD) and fluorescence (XRF) analysis and scanning electron microscopy spectral images. It is also shown how altering the chemical composition is expected to affect the furnace refractory lining. Additionally, the process has been repeated for the most suitable mix in gas furnace and physical properties (FI, SI, LA, PSV, AAV, volume stability) examined. Alteration of the specific weight can result in tailoring slag properties for specific applications in the construction sector.

  4. Oxidation Resistant Graphite Studies

    Energy Technology Data Exchange (ETDEWEB)

    W. Windes; R. Smith

    2014-07-01

    The Very High Temperature Reactor (VHTR) Graphite Research and Development Program is investigating doped nuclear graphite grades exhibiting oxidation resistance. During a oxygen ingress accident the oxidation rates of the high temperature graphite core region would be extremely high resulting in significant structural damage to the core. Reducing the oxidation rate of the graphite core material would reduce the structural effects and keep the core integrity intact during any air-ingress accident. Oxidation testing of graphite doped with oxidation resistant material is being conducted to determine the extent of oxidation rate reduction. Nuclear grade graphite doped with varying levels of Boron-Carbide (B4C) was oxidized in air at nominal 740°C at 10/90% (air/He) and 100% air. The oxidation rates of the boronated and unboronated graphite grade were compared. With increasing boron-carbide content (up to 6 vol%) the oxidation rate was observed to have a 20 fold reduction from unboronated graphite. Visual inspection and uniformity of oxidation across the surface of the specimens were conducted. Future work to determine the remaining mechanical strength as well as graphite grades with SiC doped material are discussed.

  5. Hydrophilization of graphite using plasma above/in a solution

    Science.gov (United States)

    Hoshino, Shuhei; Kawahara, Kazuma; Takeuchi, Nozomi

    2018-01-01

    A hydrophilization method for graphite is required for applications such as conductive ink. In typical chemical oxidation methods for graphite have the problems of producing many defects in graphite and a large environmental impact. In recent years, the plasma treatment has attracted attention because of the high quality of the treated samples and the low environmental impact. In this study, we proposed an above-solution plasma treatment with a high contact probability of graphite and plasma since graphite accumulates on the solution surface due to its hydrophobicity, which we compared with a so-called solution plasma treatment. Graphite was hydrophilized via reactions with OH radicals generated by the plasma. It was confirmed that hydroxyl and carboxyl groups were modified to the graphite and the dispersibility was improved. The above-solution plasma achieved more energy-efficient hydrophilization than the solution plasma and it was possible to enhance the dispersibility by increasing the plasma–solution contact area.

  6. Method for producing dustless graphite spheres from waste graphite fines

    Science.gov (United States)

    Pappano, Peter J [Oak Ridge, TN; Rogers, Michael R [Clinton, TN

    2012-05-08

    A method for producing graphite spheres from graphite fines by charging a quantity of spherical media into a rotatable cylindrical overcoater, charging a quantity of graphite fines into the overcoater thereby forming a first mixture of spherical media and graphite fines, rotating the overcoater at a speed such that the first mixture climbs the wall of the overcoater before rolling back down to the bottom thereby forming a second mixture of spherical media, graphite fines, and graphite spheres, removing the second mixture from the overcoater, sieving the second mixture to separate graphite spheres, charging the first mixture back into the overcoater, charging an additional quantity of graphite fines into the overcoater, adjusting processing parameters like overcoater dimensions, graphite fines charge, overcoater rotation speed, overcoater angle of rotation, and overcoater time of rotation, before repeating the steps until graphite fines are converted to graphite spheres.

  7. High Efficiency Solar Furnace Core Project

    Data.gov (United States)

    National Aeronautics and Space Administration — It is proposed to develop a high efficiency solar furnace core that greatly lessens the heat losses from the furnace core, either greatly reducing the amount of...

  8. Coating method for graphite

    Science.gov (United States)

    Banker, J.G.; Holcombe, C.E. Jr.

    1975-11-06

    A method of limiting carbon contamination from graphite ware used in induction melting of uranium alloys is provided. The graphite surface is coated with a suspension of Y/sub 2/O/sub 3/ particles in water containing about 1.5 to 4 percent by weight sodium carboxymethylcellulose.

  9. Terahertz generation from graphite

    NARCIS (Netherlands)

    Ramakrishnan, G.; Chakkittakandy, R.; Planken, P.C.M.

    2009-01-01

    Generation of subpicosecond terahertz pulses is observed when graphite surfaces are illuminated with femtosecond near-infrared laser pulses. The nonlinear optical generation of THz pulses from graphite is unexpected since, in principle, the material possesses a centre of inversion symmetry.

  10. Training Guidelines: Glass Furnace Operators.

    Science.gov (United States)

    Ceramics, Glass, and Mineral Products Industry Training Board, Harrow (England).

    Technological development in the glass industry is constantly directed towards producing high quality glass at low operating costs. Particularly, changes have taken place in melting methods which mean that the modern furnace operator has greater responsibilities than any of his predecessors. The complexity of control systems, melting rates, tank…

  11. Modeling energy consumption of residential furnaces and boilers in U.S. homes

    Energy Technology Data Exchange (ETDEWEB)

    Lutz, James; Dunham-Whitehead, Camilla; Lekov, Alex; McMahon, James

    2004-02-01

    In 2001, DOE initiated a rulemaking process to consider whether to amend the existing energy efficiency standards for furnaces and boilers. A key factor in DOE's consideration of new standards is their cost-effectiveness to consumers. Determining cost-effectiveness requires an appropriate comparison of the additional first cost of energy efficiency design options with the savings in operating costs. This report describes calculation of equipment energy consumption (fuel and electricity) based on estimated conditions in a sample of homes that are representative of expected furnace and boiler installations. To represent actual houses with furnaces and boilers in the United States, we used a set of houses from the Residential Energy Consumption Survey of 1997 conducted by the Energy Information Administration. Our calculation methodology estimates the energy consumption of alternative (more-efficient) furnaces, if they were to be used in each house in place of the existing equipment. We developed the method of calculation described in this report for non-weatherized gas furnaces. We generalized the energy consumption calculation for this product class to the other furnace product classes. Fuel consumption calculations for boilers are similar to those for the other furnace product classes. The electricity calculations for boilers are simpler than for furnaces, because boilers do not provide thermal distribution for space cooling as furnaces often do.

  12. Development of High-Temperature Blackbodies and Furnaces for Radiation Thermometry

    Science.gov (United States)

    Khlevnoy, B. B.; Samoylov, M. L.; Grigoryeva, I. A.; Ibragimov, N. A.; Shapoval, V. I.; Puzanov, A. V.; Ogarev, S. A.

    2011-08-01

    Two high-temperature blackbodies were developed and tested. The first one is a graphite blackbody with a maximum temperature of 2000 °C, an opening of 40 mm, and an emissivity of 0.995. It is intended for the routine calibration of pyrometers. The second one is a small version of a pyrolytic graphite (PG) blackbody with a cavity diameter of 15 mm, an opening of 10 mm, and an emissivity of 0.9996. The blackbody has two options with maximum temperatures of 2500 °C and 3000 °C, respectively. With these, the list of high-temperature blackbodies developed at VNIIOFI consists of five PG types and one graphite type, which can be used in radiation thermometry as precision Planckian sources or furnaces for fixed-point applications. The article also describes modifications to the PG furnace, where PG heater rings are replaced partly or totally by graphite elements. Such modifications extend the lifetime of the heater, reduce the cost for some applications and, for some cases, improve the temperature uniformity.

  13. Asymptomatic Intracorneal Graphite Deposits following Graphite Pencil Injury

    OpenAIRE

    Swetha Sara Philip; Deepa John; Sheeja Susan John

    2012-01-01

    Reports of graphite pencil lead injuries to the eye are rare. Although graphite is considered to remain inert in the eye, it has been known to cause severe inflammation and damage to ocular structures. We report a case of a 12-year-old girl with intracorneal graphite foreign bodies following a graphite pencil injury.

  14. Physical and mechanical properties of lamellar compounds of graphite

    OpenAIRE

    Костиков, Александр Анатольевич; Довгаль, Анна Николаевна; Черномаз, Владимир Николаевич; Кузнецов, Андрей Андреевич

    2013-01-01

    In this paper physical, mechanical and thermophysical properties of lamellar graphite compounds with various intercalants have been studied as a function of temperature and oxidants. The focus of the study was the influence of various factors on lamellar graphite compounds parameters, namely: elongation of samples, thermal expansion coefficient, thermal conductivity. The following factors have been considered: oxidant concentration in the synthesis of lamellar graphite compounds, the particle...

  15. Torrefied biomasses in a drop tube furnace to evaluate their utility in blast furnaces.

    Science.gov (United States)

    Chen, Wei-Hsin; Du, Shan-Wen; Tsai, Chien-Hsiung; Wang, Zhen-Yu

    2012-05-01

    Torrefaction and burning characteristics of bamboo, oil palm, rice husk, bagasse, and Madagascar almond were studied and compared with a high-volatile bituminous coal using a drop tube furnace to evaluate the potential of biomass consumed in blast furnaces. Torrefaction at 250 and 300°C for 1h duration was carried out. Analysis using the ash tracer method indicated that the extent of atomic carbon reduction in the biomasses was less than that of atomic hydrogen and oxygen. Torrefaction also lowered the sulfur content in bamboo and oil palm over 33%. An examination of the R-factor and burnout of the samples suggests that more volatiles were released and a higher burnout was achieved with raw and torrefied biomasses at 250°C than at 300°C; however, torrefaction at 300°C is a feasible operating condition to transform biomass into a solid fuel resembling a high-volatile bituminous coal used for blast furnaces. Copyright © 2012 Elsevier Ltd. All rights reserved.

  16. Alkaline carbonates in blast furnace process

    Directory of Open Access Journals (Sweden)

    P. Besta

    2014-10-01

    Full Text Available The production of iron in blast furnaces is a complex of physical, chemical and mechanical processes. The input raw materials contain not only metallic components, but also a number of negative elements. The most important negative elements include alkaline carbonates. They can significantly affect the course of the blast furnace process and thus the overall performance of the furnace. As a result of that, it is essential to accurately monitor the alkali content in the blast furnace raw materials. The article analyzes the alkali content in input and output raw materials and their impact on the blast furnace process.

  17. Microfabricated disposable nanosensor based on CdSe quantum dot/ionic liquid-mediated hollow fiber-pencil graphite electrode for simultaneous electrochemical quantification of uric acid and creatinine in human samples

    Energy Technology Data Exchange (ETDEWEB)

    Hooshmand, Sara; Es' haghi, Zarrin, E-mail: eshaghi@pnu.ac.ir

    2017-06-15

    In this research, a novel sensitive electrochemical nanosensor based on the cadmium selenide quantum dots (QDs)/ionic liquid mediated hollow fiber-pencil graphite electrode (HF-PGE) was prepared and applied for simultaneous determination of uric acid (UA) and creatinine (Crn) in urine and serum samples. The electrocatalytic oxidation of the analytes was investigated via differential pulse (DPV) and cyclic voltammetry (CV). The experiments were designed, in two different steps, according to Taguchi's method; OA9 L9 (3{sup 3}) and OA9 L9 (3{sup 4}) orthogonal array to optimize experimental runs. The results revealed that the electrode response was initially influenced by the types of sensor and types of ionic liquids and their ratios. The amount of QD, buffer pH, equilibration time and scan rate also influenced electrode response efficiency. According to the results of Taguchi analysis, the amount of tetra phenyl phosphonium chloride (TPPC) and QD were the most influencing parameters on the yield response of the modified electrodes. Linear ranges were obtained between 0.297–2.970 × 10{sup 3} and 0.442–8.840 × 10{sup 3} μM, with the detection limits of 0.083 and 0.229 μM and relative standard deviations (RSD) of 2.4% and 1.8%, for UA and Crn, respectively. Finally, the proposed method was successfully examined for simultaneous determination of UA and Crn in human urine and serum samples. - Highlights: • Sensor based on modified CdSe quantum dot/ionic liquid mediated hollow fiber graphite electrode. • One-step simultaneous purification, pre-concentration, extraction, back-extraction and determination of electroactive analytes. • Target analyte uric acid (UA) and creatinine (Crn) in urine and serum samples. • Disposable nature of sensor reduced risk of carry-over.

  18. Graphite for fusion energy applications

    Energy Technology Data Exchange (ETDEWEB)

    Eatherly, W.P.; Clausing, R.E.; Strehlow, R.A.; Kennedy, C.R.; Mioduszewski, P.K.

    1987-03-01

    Graphite is in widespread and beneficial use in present fusion energy devices. This report reflects the view of graphite materials scientists on using graphite in fusion devices. Graphite properties are discussed with emphasis on application to fusion reactors. This report is intended to be introductory and descriptive and is not intended to serve as a definitive information source. (JDH)

  19. Analyses of laser and furnace treated sol-gel coatings

    NARCIS (Netherlands)

    De Hosson, JT; De Haas, M; Sudarshan, TS; Jeandin, M; Khor, KA

    1998-01-01

    Here we explore a new method that allows thin films to be made with almost any composition and degree of porosity by means of a combination of sol-gel and laser technology. Results are presented for furnace and laser treated TEOTI-(tetraethylorthotitanate as sol precursor) coated silicon samples.

  20. Electroanalytical Methodology for the Direct Determination of 2,4-Dichlorophenoxyacetic Acid in Soil Samples Using a Graphite-Polyurethane Electrode

    Directory of Open Access Journals (Sweden)

    Fernanda Ramos de Andrade

    2014-01-01

    Full Text Available An electroanalytical methodology was developed for the direct determination of the herbicide 2,4-dichlorophenoxyacetic acid (2,4-D using a graphite-polyurethane composite electrode and square wave voltammetry (SWV. 2,4-D exhibited one reduction peak with characteristics of an irreversible process at −0.54 V (versus Ag/AgCl, which is controlled by the diffusion of the reagent on the electrode surface. After the experimental parameters optimization (pH 2.0, f=50 s−1, a=0.50 V, and ΔEi=0.03 V, analytical curves were constructed in the range of 0.66 mg L−1 to 2.62  mg L−1. Detection (LD and quantification (LQ limits were 17.6 μg L−1 and 58.6 μg L−1, respectively. The methodology was successfully applied to measure the percolation of the herbicide 2,4-D in undisturbed soil columns of different granulometric compositions.

  1. Fission Product Sorptivity in Graphite

    Energy Technology Data Exchange (ETDEWEB)

    Tompson, Jr., Robert V. [Univ. of Missouri, Columbia, MO (United States); Loyalka, Sudarshan [Univ. of Missouri, Columbia, MO (United States); Ghosh, Tushar [Univ. of Missouri, Columbia, MO (United States); Viswanath, Dabir [Univ. of Missouri, Columbia, MO (United States); Walton, Kyle [Univ. of Missouri, Columbia, MO (United States); Haffner, Robert [Univ. of Missouri, Columbia, MO (United States)

    2015-04-01

    graduate student meant that data acquisition with the packed bed systems ended up competing for the graduate student’s available time with the electrodynamic balance redesign and assembly portions of the project. This competition for available time was eventually mitigated to some extent by the later recruitment of an undergraduate student to help with data collection using the packed bed system. It was only the recruitment of the second student that allowed the single particle balance design and construction efforts to proceed as far as they did during the project period. It should be added that some significant time was also spent by the graduate student cataloging previous work involving graphite. This eventually resulted in a review paper being submitted and accepted (“Adsorption of Iodine on Graphite in High Temperature Gas-Cooled Reactor Systems: A Review,” Kyle L. Walton, Tushar K. Ghosh, Dabir S. Viswanath, Sudarshan K. Loyalka, Robert V. Tompson). Our specific revised objectives in this project were as follows: Experimentally obtain isotherms of Iodine for reactor grade IG-110 samples of graphite particles over a range of temperatures and pressures using an EDB and a temperature controlled EDB; Experimentally obtain isotherms of Iodine for reactor grade IG-110 samples of graphite particles over a range of temperatures and pressures using a packed column bed apparatus; Explore the effect that charge has on the adsorption isotherms of iodine by varying the charges on and the voltages used to suspend the microscopic particles in the EDB; and To interpret these results in terms of the existing models (Langmuir, BET, Freundlich, and others) which we will modify as necessary to include charge related effects.

  2. Comparison between the Strength Levels of Baseline Nuclear-Grade Graphite and Graphite Irradiated in AGC-2

    Energy Technology Data Exchange (ETDEWEB)

    Carroll, Mark Christopher [Idaho National Laboratory (INL), Idaho Falls, ID (United States)

    2015-07-01

    This report details the initial comparison of mechanical strength properties between the cylindrical nuclear-grade graphite specimens irradiated in the second Advanced Graphite Creep (AGC-2) experiment with the established baseline, or unirradiated, mechanical properties compiled in the Baseline Graphite Characterization program. The overall comparative analysis will describe the development of an appropriate test protocol for irradiated specimens, the execution of the mechanical tests on the AGC-2 sample population, and will further discuss the data in terms of developing an accurate irradiated property distribution in the limited amount of irradiated data by leveraging the considerably larger property datasets being captured in the Baseline Graphite Characterization program. Integrating information on the inherent variability in nuclear-grade graphite with more complete datasets is one of the goals of the VHTR Graphite Materials program. Between “sister” specimens, or specimens with the same geometry machined from the same sub-block of graphite from which the irradiated AGC specimens were extracted, and the Baseline datasets, a comprehensive body of data will exist that can provide both a direct and indirect indication of the full irradiated property distributions that can be expected of irradiated nuclear-grade graphite while in service in a VHTR system. While the most critical data will remain the actual irradiated property measurements, expansion of this data into accurate distributions based on the inherent variability in graphite properties will be a crucial step in qualifying graphite for nuclear use as a structural material in a VHTR environment.

  3. Oxidation Character of Carbon Composite Bricks Used in Blast Furnace

    Science.gov (United States)

    Zuo, Haibin; Wang, Cong; Zhang, Jianliang; Jiao, Kexin; Zhao, Yongan

    The carbon composite brick is a new refractory used in blast furnace hearth and bottom. It caused wide attention due to its high thermal conductivity and low erosion by molten iron. In this paper, chemical constituents, SEM-EDS and X-ray diffraction were carried out in order to understand reaction mechanisms. A series of experiments of oxidation resistance characteristics were made. The oxidation mechanisms of carbon composite bricks in the presence of air were analyzed. According to the analysis on many experimental results, the oxidation process of carbon composite bricks under different temperatures were controlled by different mechanisms. In the condition of high temperature, SiO2 as oxidation product hindered the diffusion of O2, and reduced the oxidation loss of graphite in the internal.

  4. Intercalated graphite electrical conductors

    Science.gov (United States)

    Banks, B. A.

    1983-01-01

    For years NASA has wanted to reduce the weight of spacecraft and aircraft. Experiments are conducted to find a lightweight synthetic metal to replace copper. The subject of this paper, intercalated graphite, is such a material. Intercalated graphite is made by heating petroleum or coal to remove the hydrogen and to form more covalent bonds, thus increasing the molecular weight. The coal or petroleum eventually turns to pitch, which can then be drawn into a fiber. With continued heating the pitch-based fiber releases hydrogen and forms a carbon fiber. The carbon fiber, if heated sufficiently, becomes more organized in parallel layers of hexagonally arranged carbon atoms in the form of graphite. A conductor of intercalated graphite is potentially useful for spacecraft or aircraft applications because of its low weight.

  5. Brominated graphitized carbon fibers

    Science.gov (United States)

    Hung, Ching-Cheh (Inventor)

    1991-01-01

    Low cost, high break elongation graphitized carbon fibers having low degree of graphitization are inert to bromine at room or higher temperatures, but are brominated at -7 to 20 C, and then debrominated at ambient. Repetition of this bromination-debromination process can bring the bromine content to 18 percent. Electrical conductivity of the brominated fibers is three times of the before-bromination value.

  6. Graphitized Cast Irons

    Science.gov (United States)

    Silman, G. I.; Makarenko, K. V.

    2014-05-01

    An analytical review of data on general-purpose grayed cast iron with different forms of graphite (lamellar, vermicular, globular, flaked) is presented. Grades of cast iron, their compositions, special features of structure of the graphite, and properties of gray, high-strength and malleable irons are described. The data on the kinds of iron considered are compared with those stipulated in international and some national standards.

  7. Microstructure transition from lamellar to compacted graphite using different modification agents

    Energy Technology Data Exchange (ETDEWEB)

    Geier, G.F. [Austrian Foundry Research Institute, Parkstrasse 21, 8700 Leoben (Austria)]. E-mail: geier.ogi@unileoben.ac.at; Bauer, W. [Austrian Foundry Research Institute, Parkstrasse 21, 8700 Leoben (Austria); McKay, B.J. [University of Leoben, Lehrstuhl fuer Giessereikunde, Franz-Josef-St. 18, 8700 Leoben (Austria); Schumacher, P. [Austrian Foundry Research Institute, Parkstrasse 21, 8700 Leoben (Austria); University of Leoben, Lehrstuhl fuer Giessereikunde, Franz-Josef-St. 18, 8700 Leoben (Austria)

    2005-12-15

    The graphite morphology present in compacted graphite irons can vary between a spheroidal and lamellar range of shapes. These graphite shapes have been studied by scanning electron microscopy (SEM). Samples used were treated either with magnesium, cerium or lanthanum to investigate differences in the modification of the graphite structure between each of these elements. To facilitate the SEM study the samples were deep etched to reveal the graphite structure in three dimensions. Results showed that there was little difference between the morphologies displayed in the well-formed compacted graphite. However, the lamellar graphite formed varied considerably with each of the three modification agents. The transition from compacted to lamellar shape was continuous for Mg treatment, whereas there was a sharp transition when treated with rare earth elements. Furthermore, several degenerated graphite structures in the La-treated sample were observed.

  8. Behavior of an indigenously fabricated transferred arc plasma furnace for smelting studies

    Science.gov (United States)

    A, K. MANDAL; R, K. DISHWAR; O, P. SINHA

    2018-03-01

    The utilization of industrial solid waste for metal recovery requires high-temperature tools due to the presence of silica and alumina, which is reducible at high temperature. In a plasma arc furnace, transferred arc plasma furnace (TAP) can meet all requirements, but the disadvantage of this technology is the high cost. For performing experiments in the laboratory, the TAP was fabricated indigenously in a laboratory based on the different inputs provided in the literature for the furnace design and fabrication. The observed parameters such as arc length, energy consumption, graphite electrode consumption, noise level as well as lining erosion were characterized for this fabricated furnace. The nitrogen plasma increased by around 200 K (200 °C) melt temperature and noise levels decreased by ∼10 dB compared to a normal arc. Hydrogen plasma offered 100 K (100 °C) higher melt temperature with ∼5 dB higher sound level than nitrogen plasma. Nitrogen plasma arc melting showed lower electrode and energy consumption than normal arc melting, whereas hydrogen plasma showed lower energy consumption and higher electrode consumption in comparison to nitrogen plasma. The higher plasma arc temperature resulted in a shorter meltdown time than normal arc with smoother arcing. Hydrogen plasma permitted more heats, reduced meltdown time, and lower energy consumption, but with increased graphite consumption and crucible wear. The present study showed that the fabricated arc plasma is better than the normal arc furnace with respect to temperature generation, energy consumption, and environmental friendliness. Therefore, it could be used effectively for smelting-reduction studies.

  9. From anthracites to graphite: influences of temperature, pressure and shear

    Energy Technology Data Exchange (ETDEWEB)

    Beyssac, O.; Goffe, B.; Rouzaud, J.-N.; Clinard, C.; Cassareuil, J.; Catel, N. [Ecole Normale Superieure, Paris (France). Laboratoire de Geologie

    1999-07-01

    In order to study natural graphitization, a homogenous series of organic matter bearing metasediments were sampled. The structural and microtextural evolution of organic matter was followed using Raman spectroscopy and transmission electron microscopy. Natural graphitization was shown to be enhanced by temperature, pressure and shear. 9 refs., 2 figs.

  10. Glass Furnace Combustion and Melting Research Facility.

    Energy Technology Data Exchange (ETDEWEB)

    Connors, John J. (PPG Industries, Inc., Pittsburgh, PA); McConnell, John F. (JFM Consulting, Inc., Pittsburgh, PA); Henry, Vincent I. (Henry Technology Solutions, LLC, Ann Arbor, MI); MacDonald, Blake A.; Gallagher, Robert J.; Field, William B. (Lilja Corp., Livermore, CA); Walsh, Peter M.; Simmons, Michael C. (Lilja Corp., Livermore, CA); Adams, Michael E. (Lilja Corp., Rochester, NY); Leadbetter, James M. (A.C. Leadbetter and Son, Inc., Toledo, OH); Tomasewski, Jack W. (A.C. Leadbetter and Son, Inc., Toledo, OH); Operacz, Walter J. (A.C. Leadbetter and Son, Inc., Toledo, OH); Houf, William G.; Davis, James W. (A.C. Leadbetter and Son, Inc., Toledo, OH); Marvin, Bart G. (A.C. Leadbetter and Son, Inc., Toledo, OH); Gunner, Bruce E. (A.C. Leadbetter and Son, Inc., Toledo, OH); Farrell, Rick G. (A.C. Leadbetter and Son, Inc., Toledo, OH); Bivins, David P. (PPG Industries, Inc., Pittsburgh, PA); Curtis, Warren (PPG Industries, Inc., Pittsburgh, PA); Harris, James E. (PPG Industries, Inc., Pittsburgh, PA)

    2004-08-01

    solution of proprietary glass production problems. As a consequence of the substantial increase in scale and scope of the initial furnace concept in response to industry recommendations, constraints on funding of industrial programs by DOE, and reorientation of the Department's priorities, the OIT Glass Program is unable to provide the support for construction of such a facility. However, it is the present investigators' hope that a group of industry partners will emerge to carry the project forward, taking advantage of the detailed furnace design presented in this report. The engineering, including complete construction drawings, bill of materials, and equipment specifications, is complete. The project is ready to begin construction as soon as the quotations are updated. The design of the research melter closely follows the most advanced industrial practice, firing by natural gas with oxygen. The melting area is 13 ft x 6 ft, with a glass depth of 3 ft and an average height in the combustion space of 3 ft. The maximum pull rate is 25 tons/day, ranging from 100% batch to 100% cullet, continuously fed, with variable batch composition, particle size distribution, and raft configuration. The tank is equipped with bubblers to control glass circulation. The furnace can be fired in three modes: (1) using a single large burner mounted on the front wall, (2) by six burners in a staggered/opposed arrangement, three in each breast wall, and (3) by down-fired burners mounted in the crown in any combination with the front wall or breast-wall-mounted burners. Horizontal slots are provided between the tank blocks and tuck stones and between the breast wall and skewback blocks, running the entire length of the furnace on both sides, to permit access to the combustion space and the surface of the glass for optical measurements and sampling probes. Vertical slots in the breast walls provide additional access for measurements and sampling. The furnace and tank are to be fully

  11. Solid-phase extraction of polar pesticides from environmental water samples on graphitized carbon and Empore-activated carbon disks and on-line coupling to octadecyl-bonded silica analytical columns.

    Science.gov (United States)

    Slobodník, J; Oztezkizan, O; Lingeman, H; Brinkman, U A

    1996-10-25

    The suitability of Empore-activated carbon disks (EACD), Envi-Carb graphitized carbon black (GCB) and CPP-50 graphitized carbon for the trace enrichment of polar pesticides from water samples was studied by means of off-line and on-line solid-phase extraction (SPE). In the off-line procedure, 0.5-2 l samples spiked with a test mixture of oxamyl, methomyl and aldicarb sulfoxide were enriched on EnviCarb SPE cartridges or 47 mm diameter EACD and eluted with dichloromethane-methanol. After evaporation, a sample was injected onto a C18-bonded silica column and analysed by liquid chromatography with ultraviolet (LC-UV) detection. EACD performed better than EnviCarb cartridges in terms of breakthrough volumes (> 2 l for all test analytes), reproducibility (R.S.D. of recoveries, 4-8%, n = 3) and sampling speed (100 ml/min); detection limits in drinking water were 0.05-0.16 microgram/l. In the on-line experiments, 4.6 mm diameter pieces cut from original EACD and stacked onto each other in a 9 mm long precolumn, and EnviCarb and CPP-50 packed in 10 x 2.0 mm I.D. precolumn, were tested, and 50-200 ml spiked water samples were preconcentrated. Because of the peak broadening caused by the strong sorption of the analytes on carbon, the carbon-packed precolumns were eluted by a separate stream of 0.1 ml/min acetonitrile which was mixed with the gradient LC eluent in front of the C18 analytical column. The final on-line procedure was also applied for the less polar propoxur, carbaryl and methiocarb. EnviCarb could not be used due to its poor pressure resistance. CPP-50 provided less peak broadening than EACD: peak widths were 0.1-0.3 min and R.S.D. of peak heights 4-14% (n = 3). In terms of analyte trapping efficiency on-line SPE-LC-UV with a CPP-50 precolumn also showed better performance than when Bondesil C18/OH or polymeric PLRP-S was used, but chromatographic resolution was similar. With the CPP-50-based system, detection limits of the test compounds were 0.05-1 microgram

  12. Reactivity of lithium exposed graphite surface

    Science.gov (United States)

    Harilal, S. S.; Allain, J. P.; Hassanein, A.; Hendricks, M. R.; Nieto-Perez, M.

    2009-07-01

    Lithium as a plasma-facing component has many attractive features in fusion devices. We investigated chemical properties of the lithiated graphite surfaces during deposition using X-ray photoelectron spectroscopy and low-energy ion scattering spectroscopy. In this study we try to address some of the known issues during lithium deposition, viz., the chemical state of lithium on graphite substrate, oxide layer formation mechanisms, Li passivation effects over time, and chemical change during exposure of the sample to ambient air. X-ray photoelectron studies indicate changes in the chemical composition with various thickness of lithium on graphite during deposition. An oxide layer formation is noticed during lithium deposition even though all the experiments were performed in ultrahigh vacuum. The metal oxide is immediately transformed into carbonate when the deposited sample is exposed to air.

  13. Reactivity of lithium exposed graphite surface

    Energy Technology Data Exchange (ETDEWEB)

    Harilal, S.S., E-mail: sharilal@purdue.edu [Purdue University, School of Nuclear Engineering, 400 Central Dr., West Lafayette, IN 47907 (United States); Allain, J.P.; Hassanein, A. [Purdue University, School of Nuclear Engineering, 400 Central Dr., West Lafayette, IN 47907 (United States); Hendricks, M.R. [Argonne National Laboratory, 9700 S. Cass Avenue, Argonne, IL 60439 (United States); Nieto-Perez, M. [CICATA-IPN, Cerro Blanco 141 Cimatario, Queretaro QRO 76090 (Mexico)

    2009-07-30

    Lithium as a plasma-facing component has many attractive features in fusion devices. We investigated chemical properties of the lithiated graphite surfaces during deposition using X-ray photoelectron spectroscopy and low-energy ion scattering spectroscopy. In this study we try to address some of the known issues during lithium deposition, viz., the chemical state of lithium on graphite substrate, oxide layer formation mechanisms, Li passivation effects over time, and chemical change during exposure of the sample to ambient air. X-ray photoelectron studies indicate changes in the chemical composition with various thickness of lithium on graphite during deposition. An oxide layer formation is noticed during lithium deposition even though all the experiments were performed in ultrahigh vacuum. The metal oxide is immediately transformed into carbonate when the deposited sample is exposed to air.

  14. Fabrication of novel coated pyrolytic graphite electrodes for the selective nano-level monitoring of Cd²⁺ ions in biological and environmental samples using polymeric membrane of newly synthesized macrocycle.

    Science.gov (United States)

    Sahani, Manoj Kumar; Singh, A K; Jain, A K; Upadhyay, Anjali; Kumar, Amit; Singh, Udai P; Narang, Shikha

    2015-02-20

    Novel 5-amino-1,3,4-thiadiazole-2-thiol unit based macrocyclic ionophore 5,11,17-trithia-1,3,7,9,13,15,19,20,21-nonaazatetracyclo[14.2.1.1(4,7).1(10,13)]henicosa-4(20),10(21),16(19)-triene-6,12,18-trithione (M1), was synthesized and characterized. Preliminary studies on M1 have showed that it has more the affinity toward Cd(2+) ion. Thus, the macrocyclic ionophore (M1) was used as electroactive material in the fabrication of PVC-membrane electrodes such as polymeric membrane electrode (PME), coated graphite electrode (CGE) and coated pyrolytic graphite electrode (CPGE) were prepared and its performance characteristic were compared with. The electroanalytical studies performed on PME, CGE and CPGE revealed that CPGE having membrane composition M1:PVC:1-CN:NaTPB in the ratio of 7:37:54:2 exhibits the best potentiometric characteristics in terms of detection limit of 7.58×10(-9) mol L(-1), Nernstian slope of 29.6 mV decade(-1) of activity. The sensor was found to be independent of pH in the range 2.5-8.5. The sensor showed a fast response time of 10s and could be used over a period of 4 months without any significant divergence in its potentiometric characteristics. The sensor has been employed for monitoring of the Cd(2+) ion in real samples and also used as an indicator electrode in the potentiometric titration of Cd(2+) ion with EDTA. Copyright © 2014. Published by Elsevier B.V.

  15. A bench arc-furnace facility for fullerene and single-wall nanotubes synthesis

    Directory of Open Access Journals (Sweden)

    Huber John G

    2001-01-01

    Full Text Available A metallic-sample arc-furnace was modified to synthesize fullerenes and nanotubes. The (reversible changes and the process for producing single-wall nanotubes (SWNTs are described.

  16. Contamination-free graphene by chemical vapor deposition in quartz furnaces

    National Research Council Canada - National Science Library

    Nicola Lisi; Theodoros Dikonimos; Francesco Buonocore; Martina Pittori; Raffaello Mazzaro; Rita Rizzoli; Sergio Marras; Andrea Capasso

    2017-01-01

    .... When graphene is grown in quartz furnaces, in particular, it is common to end up with samples contaminated by heterogeneous particles, which alter the growth mechanism and affect graphene’s properties...

  17. Electron dynamics in MoS2-graphite heterostructures.

    Science.gov (United States)

    Zhang, Xinwu; He, Dawei; Yi, Lixin; Zhao, Siqi; He, Jiaqi; Wang, Yongsheng; Zhao, Hui

    2017-10-05

    The electron dynamics in heterostructures formed by multilayer graphite and monolayer or bulk MoS2 were studied by femtosecond transient absorption measurements. Samples of monolayer MoS2-multilayer graphite and bulk MoS2-multilayer graphite were fabricated by exfoliation and dry transfer techniques. Ultrafast laser pulses were used to inject electron-hole pairs into monolayer or bulk MoS2. The transfer of these photocarriers to the adjacent multilayer graphite was time resolved by measuring the differential reflection of a probe pulse. We found that photocarriers injected into monolayer MoS2 transfer to graphite on an ultrafast time scale shorter than 400 fs. Such an efficient charge transfer is key to the development of high performance optoelectronic devices with MoS2 as the light absorbing layer and graphite as electrodes. The absorption coefficient of monolayer MoS2 can be controlled by the carriers in graphite. This process can be used for interlayer coupling and control. In a bulk MoS2-graphite heterostructure, the photocarrier transfer time is about 220 ps, due to the inefficient interlayer charge transport in bulk MoS2. These results provide useful information for developing optoelectronic devices based on MoS2-graphite heterostructures.

  18. Measurement of airflow in residential furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Biermayer, Peter J.; Lutz, James; Lekov, Alex

    2004-01-24

    In order to have a standard for furnaces that includes electricity consumption or for the efficiency of furnace blowers to be determined, it is necessary to determine the airflow of a furnace or furnace blower. This study focused on airflow testing, in order to determine if an existing test method for measuring blower airflow could be used to measure the airflow of a furnace, under conditions seen in actual installations and to collect data and insights into the operating characteristics of various types of furnace blowers, to use in the analysis of the electricity consumption of furnaces. Results of the measured airflow on furnaces with three types of blower and motor combinations are presented in the report. These included: (1) a forward-curved blower wheel with a typical permanent split capacitor (PSC) motor, (2) a forward-curved blower wheel with an electronically-commutated motor (ECM), and (3) a prototype blower, consisting of a backward-inclined blower wheel matched to an ECM motor prototype, which is being developed as an energy-saving alternative to conventional furnace blowers. The testing provided data on power consumption, static and total pressure, and blower speed.

  19. Recompressed exfoliated graphite articles

    Science.gov (United States)

    Zhamu, Aruna; Shi, Jinjun; Guo, Jiusheng; Jang, Bor Z

    2013-08-06

    This invention provides an electrically conductive, less anisotropic, recompressed exfoliated graphite article comprising a mixture of (a) expanded or exfoliated graphite flakes; and (b) particles of non-expandable graphite or carbon, wherein the non-expandable graphite or carbon particles are in the amount of between about 3% and about 70% by weight based on the total weight of the particles and the expanded graphite flakes combined; wherein the mixture is compressed to form the article having an apparent bulk density of from about 0.1 g/cm.sup.3 to about 2.0 g/cm.sup.3. The article exhibits a thickness-direction conductivity typically greater than 50 S/cm, more typically greater than 100 S/cm, and most typically greater than 200 S/cm. The article, when used in a thin foil or sheet form, can be a useful component in a sheet molding compound plate used as a fuel cell separator or flow field plate. The article may also be used as a current collector for a battery, supercapacitor, or any other electrochemical cell.

  20. Coke reactivity under blast furnace condition and in the CSR/CRI test

    OpenAIRE

    Lundgren, Maria; Björkman, Bo; Sundqvist Ökvist, Lena

    2008-01-01

    The present work aims to study the high-temperature strength of coke. Mechanisms of disintegration were evaluated using basket samples charged into LKAB's experimental blast furnace prior to quenching and dissection. Coke charged into basket samples were analysed with CSR/CRI tests and compared with treated coke from the blast furnace. Results from tumbling tests, chemical analyses of coarse and fine material, as well as light optical microscopy studies of original and treated coke have been ...

  1. Cesium diffusion in graphite

    Energy Technology Data Exchange (ETDEWEB)

    Evans, R.B. III; Davis, W. Jr.; Sutton, A.L. Jr.

    1980-05-01

    Experiments on diffusion of /sup 137/Cs in five types of graphite were performed. The document provides a completion of the report that was started and includes a presentation of all of the diffusion data, previously unpublished. Except for data on mass transfer of /sup 137/Cs in the Hawker-Siddeley graphite, analyses of experimental results were initiated but not completed. The mass transfer process of cesium in HS-1-1 graphite at 600 to 1000/sup 0/C in a helium atmosphere is essentially pure diffusion wherein values of (E/epsilon) and ..delta..E of the equation D/epsilon = (D/epsilon)/sub 0/ exp (-..delta..E/RT) are about 4 x 10/sup -2/ cm/sup 2//s and 30 kcal/mole, respectively.

  2. Materials treatment at solar furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, D.

    2002-07-01

    In the modern age, beginning in the fifties, solar furnaces have been used as a tool for research in materials technologies and treatment, as well as chemical reactor test beds. However, this is not the first time man has attempted to use sunlight as a means of manipulating the materials that surround us. During the Renaissance, Leonardo da Vinci proposed the construction of a six-kilometer parabolic mirror able to heat any boiler for a dye factory and the sculptor Andrea del Verrochio used a solar mirror to weld the parts of a spherical copper support for a lantern at Santa Maria del Fiore in Florence. At present, the materials treatment work in solar furnaces may be summarized as follows: the study of physical-thermal properties of materials at high temperatures-innovative treatments impossible to carry out with the conventional manufacturing processes, which improve certain properties of materials that are going to work under very severe conditions improving the results of industrial materials treatments such as laser surface tempering testing under laboratory conditions of materials which will have to undergo extreme conditions at high temperatures (ceramic coating of aircraft and space vehicles, turbine blades, power brake discs, electrical contacts, nuclear reactors, etc.) With regard to high temperature chemical applications, experiments are being carried out in detoxification, gasification of solid fuels, chemical reaction kinetics studies and direct absorption particle reactors. (Author) 31 refs.

  3. Materials treatment at Solar Furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, D. [Ciemat. Plataforma Solar de Almeria. Almeria (Spain)

    2000-07-01

    In the modern age, beginning in the fifties, solar furnaces have been used as a tool for research in materials technologies and treatment, as well as chemical reactor test beds. However, this is not the first time man has attempted to use sunlight as a means of manipulating the materials that surround us. During the Renaissance, Leonardo da Vinci proposed the construction of a six-kilometer parabolic mirror able to heat any boiler for a dye factory and the sculptor Andrea del Verrochio used a solar mirror to weld the parts of a spherical copper support for a lantern at Santa Maria del Fiore in Florence. At present, the materials treatment work in solar furnaces may be summarized as follows: -the study of physical-thermal properties of materials at high temperatures -innovative treatments impossible to carry out with the conventional manufacturing processes, which improve certain properties of materials that are going to work under very severe conditions -improving the results of industrial materials treatments such as laser surface tempering -testing under laboratory conditions of materials which will have to undergo extreme conditions at high temperatures (ceramic coating of aircraft and space vehicles, turbine blades, power brake discs, electrical contacts, nuclear reactors, etc.) With regard to high temperature chemical applications, experiments are being carried out in detoxification, gasification of solid fuels, chemical reaction kinetics studies and direct absorption particle reactors. (Author) 31 refs.

  4. The development of two new KC-135 furnaces for studies on microgravity materials processing

    Science.gov (United States)

    Fiske, Michael; Cockburn, James; Poorman, Richard

    1988-01-01

    Wyle Laboratories is currently designing and fabricating two KC-135 materials processing furnaces for Marshall Space Flight Center. The first of these, called the Rapid Melt/Rapid Quench (RM/RQ) Furnace, will be used to melt and resolidify Cu-, Al-, and Ni-based alloys and composites, all during the 20 to 30 seconds of low gravity (0.1 to 0.001 g) available in a single parabola of the KC-135. In addition, it will be capable of directional solidification of these alloys. The furnace can be configured for either liquid or gas quenching of the samples. The second furnace, called the Polymer Solidification Transparent (PST) Furnace, will use a wide range of sample translation rates to directionally solidify polymers and low-melting-point metals as the KC-135 flies a series of parabolic maneuvers. The use of transparent crucibles and an optics system between the hot and cold zones of the furnace will allow for high-resolution video monitoring of the solid-liquid interface during processing. It is hoped that the development of these two furnaces will lead to significant increases in understanding of interface kinetics, fluid flow, and heat transfer in materials during solidification in a low-gravity environment.

  5. Magnetic frustration of graphite oxide

    OpenAIRE

    Dongwook Lee; Jiwon Seo

    2017-01-01

    Delocalized ? electrons in aromatic ring structures generally induce diamagnetism. In graphite oxide, however, ? electrons develop ferromagnetism due to the unique structure of the material. The ? electrons are only mobile in the graphitic regions of graphite oxide, which are dispersed and surrounded by sp 3-hybridized carbon atoms. The spin-glass behavior of graphite oxide is corroborated by the frequency dependence of its AC susceptibility. The magnetic susceptibility data exhibit a negativ...

  6. Graphite-based photovoltaic cells

    Science.gov (United States)

    Lagally, Max; Liu, Feng

    2010-12-28

    The present invention uses lithographically patterned graphite stacks as the basic building elements of an efficient and economical photovoltaic cell. The basic design of the graphite-based photovoltaic cells includes a plurality of spatially separated graphite stacks, each comprising a plurality of vertically stacked, semiconducting graphene sheets (carbon nanoribbons) bridging electrically conductive contacts.

  7. Refractory of Furnaces to Reduce Environmental Impact

    Energy Technology Data Exchange (ETDEWEB)

    Hanzawa, Shigeru, E-mail: hanzawa@ngk.co.jp [NGK Insulators, LTD., Mizuho, Nagoya (Japan)

    2011-10-29

    The energy load of furnaces used in the manufacturing process of ceramics is quite large. Most of the environmental impact of ceramics manufacturing is due to the CO{sub 2} produced from this high energy load. To improve this situation, R and D has focused on furnace systems and techniques of control in order to reduce energy load. Since furnaces are comprised of refractory, consideration of their mechanical and thermal characteristics is important. Herein are described several refractory types which were chosen through comparison of the characteristics which contribute to heat capacity reduction, heat insulating reinforcement and high emissivity, thereby improving thermal radiation heat transfer efficiency to the ceramic articles. One selected refractory material which will reduce the environmental impact of a furnace, chosen considering low heat capacity and high emissivity characteristics, is SiC. In this study, thermal radiation heat transfer efficiency improvement and its effect on ceramic articles in the furnace and oxidation behaviour were investigated at 1700K. A high density SiC refractory, built into the furnace at construction, has relatively high oxidation durability and has the ability to reduce environmental impact-CO{sub 2} by 10 percent by decreasing the furnace's energy load. However, new oxidation prevention techniques for SiC will be necessary for long-term use in industrial furnaces, because passive to active oxidation transition behaviour of commercial SiC refractory is coming to close ideal.

  8. The thermal treatment of electric arc furnace dust under low gas phase pressure

    Directory of Open Access Journals (Sweden)

    W. Derda

    2009-04-01

    Full Text Available The paper presents the results of laboratory tests on the process of thermal reduction of electric arc furnace dust (EAFD in the temperature range from 1273 to 1473 K. Before proceeding to the experimental tests, a thermodynamic analysis was made using the computer program FactSage® with the aim of determining the optimal conditions for the dust components reduction reaction to proceed. The results of tests carried out, respectively, under atmospheric pressure conditions and under reduced pressure conditions are presented, where carbon in the form of graphite and blast-furnace dust (containing approx. 40 % of carbon was used as the reducer. The test results represent the effect of reduced pressure on the potential for intensifying the process of zinc removal from the dust. The degree of zinc extraction was considerably higher compared to the results of tests carried out under atmospheric pressure conditions.

  9. Determination of N-nitrosodiethanolamine, NDELA in cosmetic ingredients and products by mixed mode solid phase extraction and UPLC-tandem mass spectrometry with porous graphitic carbon column through systemic sample pre-cleanup procedure.

    Science.gov (United States)

    Joo, Kyung-Mi; Shin, Mi-Sook; Jung, Ji-hee; Kim, Boo-Min; Lee, John-Whan; Jeong, Hye-Jin; Lim, Kyung-Min

    2015-05-01

    A rapid, sensitive, accurate and specific ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method for the detection of N-nitrosodiethanolamine (NDELA), a highly toxic contaminant in cosmetic raw materials and products was developed and validated. Systematized sample preparation steps were developed according to product types. Various SPE cartridges and columns were examined to establish the condition of SPE and chromatographic separation for NDELA. Sample cleanup steps consisting of solvent and liquid-liquid extraction tailored to the various sample matrix types were established prior to mixed mode SPE (Bond Elut AccuCAT). Chromatographic separation was achieved within 7 min on a porous graphitic carbon (PGC) column using a gradient elution with the mobile phase of 1mM ammonium acetate containing 0.1% acetic acid and methanol. NDELA was monitored using an electrospray positive ionization mass spectrometry in the multiple reaction monitoring (MRM) mode (m/z 134.9>103.7(quantifier) and 73.7(qualifier ion)) with d8-NDELA (m/z 143.1>111.0) as internal standard. The standard curves were linear over the concentration range of 1-100 ng/mL with a correlation coefficient higher than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) was 10 and 20 μg/kg, respectively (0.5 and 1 ng/mL in standard solution). The intra- and inter-day precisions were estimated to be below 11.1% and accuracies were within the range of 90.8-115.8%. The validated method was successfully applied to the analysis of real samples including raw materials, skin care, make-up, shampoos and hair products. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. (Irradiation creep of graphite)

    Energy Technology Data Exchange (ETDEWEB)

    Kennedy, C.R.

    1990-12-21

    The traveler attended the Conference, International Symposium on Carbon, to present an invited paper, Irradiation Creep of Graphite,'' and chair one of the technical sessions. There were many papers of particular interest to ORNL and HTGR technology presented by the Japanese since they do not have a particular technology embargo and are quite open in describing their work and results. In particular, a paper describing the failure of Minor's law to predict the fatigue life of graphite was presented. Although the conference had an international flavor, it was dominated by the Japanese. This was primarily a result of geography; however, the work presented by the Japanese illustrated an internal program that is very comprehensive. This conference, a result of this program, was better than all other carbon conferences attended by the traveler. This conference emphasizes the need for US participation in international conferences in order to stay abreast of the rapidly expanding HTGR and graphite technology throughout the world. The United States is no longer a leader in some emerging technologies. The traveler was surprised by the Japanese position in their HTGR development. Their reactor is licensed and the major problem in their graphite program is how to eliminate it with the least perturbation now that most of the work has been done.

  11. Deconstructing graphite: graphenide solutions.

    Science.gov (United States)

    Pénicaud, Alain; Drummond, Carlos

    2013-01-15

    Growing interest in graphene over past few years has prompted researchers to find new routes for producing this material other than mechanical exfoliation or growth from silicon carbide. Chemical vapor deposition on metallic substrates now allows researchers to produce continuous graphene films over large areas. In parallel, researchers will need liquid, large scale, formulations of graphene to produce functional graphene materials that take advantage of graphene's mechanical, electrical, and barrier properties. In this Account, we describe methods for creating graphene solutions from graphite. Graphite provides a cheap source of carbon, but graphite is insoluble. With extensive sonication, it can be dispersed in organic solvents or water with adequate additives. Nevertheless, this process usually creates cracks and defects in the graphite. On the other hand, graphite intercalation compounds (GICs) provide a means to dissolve rather than disperse graphite. GICS can be obtained through the reaction of alkali metals with graphite. These compounds are a source of graphenide salts and also serve as an excellent electronic model of graphene due to the decoupling between graphene layers. The graphenide macroions, negatively charged graphene sheets, form supple two-dimensional polyelectrolytes that spontaneously dissolve in some organic solvents. The entropic gain from the dissolution of counterions and the increased degrees of freedom of graphene in solution drives this process. Notably, we can obtain graphenide solutions in easily processable solvents with low boiling points such as tetrahydrofuran or cyclopentylmethylether. We performed a statistical analysis of high resolution transmission electronic micrographs of graphene sheets deposited on grids from GICs solution to show that the dissolved material has been fully exfoliated. The thickness distribution peaks with single layers and includes a few double- or triple-layer objects. Light scattering analysis of the

  12. Graphitization of oil palm trunk chip with controlled heating condition

    Science.gov (United States)

    Karim, N. A.; Ghazali, C. M. R.; Ramli, M. M.; Halin, D. S. C.; Nainggolan, I.

    2017-09-01

    The purpose of this study is to synthesize the synthetic graphite from oil palm trunk at lower temperature (various heating temperatures, 500 °C, 800 °C and 1,000 °C) with controlled condition and study the physical properties and characterization of the graphite obtained. After heat treatment process, the samples were characterized by X-Ray Diffraction (XRD) and analyzed using X'Pert Highscore Plus software. The morphological study was carried out by using Field Emission Electro Scanning Microscope (FESEM). Based on the analysis, by heating of the sample at 800 °C, the amorphous carbon and nanocrystalline graphite were observed.

  13. Magnetic frustration of graphite oxide

    Science.gov (United States)

    Lee, Dongwook; Seo, Jiwon

    2017-03-01

    Delocalized π electrons in aromatic ring structures generally induce diamagnetism. In graphite oxide, however, π electrons develop ferromagnetism due to the unique structure of the material. The π electrons are only mobile in the graphitic regions of graphite oxide, which are dispersed and surrounded by sp3-hybridized carbon atoms. The spin-glass behavior of graphite oxide is corroborated by the frequency dependence of its AC susceptibility. The magnetic susceptibility data exhibit a negative Curie temperature, field irreversibility, and slow relaxation. The overall results indicate that magnetic moments in graphite oxide slowly interact and develop magnetic frustration.

  14. Intercalating oleylamines in graphite oxide.

    Science.gov (United States)

    Yang, Kaikun; Liang, Si; Zou, Lianfeng; Huang, Liwei; Park, Cheol; Zhu, Lisheng; Fang, Jiye; Fu, Qiang; Wang, Howard

    2012-02-07

    Graphite oxide has been synthesized from raw graphite particles and been treated with various mass amounts of oleylamine as intercalants to form intercalation compounds. X-ray diffraction patterns reveal that the inter-sheet distances strongly depend on the graphite oxide to oleylamine mass ratios. The equilibrium-like behavior implies diffusion-dominated oleylamine adsorption on graphite oxide in solution and excluded volume intercalations among oleylamine-adsorbed graphite oxide during restacking. The intercalation compounds are soluble in organic solvents, and their applications in the fabrication of transparent and conductive coatings have been demonstrated.

  15. [Determination of Al, Be, Cd, Co, Cr, Mn, Ni, Pb, Se and Tl in whole blood by atomic absorption spectrometry without preliminary sample digestion].

    Science.gov (United States)

    Ivanenko, N B; Ivanenko, A A; Solov'ev, N D; Navolotskiĭ, D V; Pavlova, O V; Ganeev, A A

    2014-01-01

    Methods of whole blood trace element determination by Graphite furnace atomic absorption spectrometry (in the variant of Zeeman's modulation polarization spectrometry) have been proposed. They do not require preliminary sample digestion. Furnace programs, modifiers and blood dilution factors were optimized. Seronorm™ human whole blood reference materials were used for validation. Dynamic ranges (for undiluted blood samples) were: Al 8 ¸ 210 мg/L; Be 0.3 ¸ 50 мg/L; Cd 0.2 ¸ 75 мg/L; Сo 5 ¸ 350 мg/L; Cr 10 ¸ 100 мg/L; Mn 6 ¸ 250 мg/L; Ni 10 ¸ 350 мg/L; Pb 3 ¸ 240 мg/L; Se 10 ¸ 500 мg/L; Tl 2 ¸ 600 мg/L. Precision (RSD) for the middle of dynamic range ranged from 5% for Mn to 11 for Se.

  16. Fast heating induced impulse halogenation of refractory sample components in electrothermal atomic absorption spectrometry by direct injection of a liquid halogenating agent.

    Science.gov (United States)

    György, Krisztina; Ajtony, Zsolt; Van Meel, Katleen; Van Grieken, René; Czitrovszky, Aladár; Bencs, László

    2011-09-15

    A novel electrothermal atomic absorption spectrometry (ETAAS) method was developed for the halogenation of refractory sample components (Er, Nd and Nb) of lithium niobate (LiNbO(3)) and bismuth tellurite (Bi(2)TeO(5)) optical single crystals to overcome memory effects and carry-over. For this purpose, the cleaning step of a regular graphite furnace heating program was replaced with a halogenation cycle. In this cycle, after the graphite tube cooled to room temperature, a 20 μL aliquot of liquid carbon tetrachloride (CCl(4)) was dispensed with a conventional autosampler into the graphite tube. The CCl(4) was partially dried at 80°C under the mini-flow (40 cm(3) min(-1)) condition of the Ar internal furnace gas (IFG), then the residue was decomposed (pyrolyzed) by fast furnace heating at 1900-2100°C under interrupted flow of the IFG. This step was followed by a clean-out stage at 2100°C under the maximum flow of the IFG. The advantage of the present method is that it does not require any alteration to the graphite furnace gas supply system in contrast to most of the formerly introduced halogenation techniques. The effectiveness of the halogenation method was verified with the determination of Er and Nd dopants in the optical crystals. In these analyses, a sensitivity decrease was observed, which was likely due to the enhanced deterioration of the graphite tube surface. Therefore, the application of mathematical correction (resloping) of the calibration was also required. The calibration curves were linear up to 1.5 and 10 μmol L(-1) for Er and Nd, respectively. Characteristic masses of 18 and 241 pg and the limit of detection (LOD) values of 0.017 and 0.27 μmol L(-1) were found for Er and Nd, respectively. These LOD data correspond to 0.68 μmol mol(-1) Er and 11 μmol mol(-1) Nd in solid bismuth tellurite samples. The analytical results were compared with those obtained by a conventional ETAAS method and validated with X-ray fluorescence spectrometry analysis

  17. Acoustic characteristics of electric arc furnaces

    Science.gov (United States)

    Cherednichenko, V. S.; Bikeev, R. A.; Cherednichenko, A. V.; Ognev, A. M.

    2016-06-01

    A mathematical model is constructed to describe the appearance and development of the noise characteristics of superpower electric arc furnaces. The noise formation is shown to be related to the pulsation of the axial plasma flows in arc discharges because of the electrodynamic pressure oscillations caused by the interaction of the self-magnetic field with the current passing in an arc. The pressure in the arc axis changes at a frequency of 100 Hz at the maximum operating pressure of 66 kPa for an arc current of 80 kA. The main ac arc sound frequencies are multiples of 100 Hz, which is supported in the practice of operation of electric arc furnaces. The sound intensity in the furnace laboratory reaches 160 dB and is decreased to 115-120 dB in the working furnace area due to shielding by the furnace jacket, the molten metal, and the molten slag. The appropriateness of increasing the hermetic sealing of electric furnaces and creating furnaces operating at low currents and high transformer voltages is corroborated.

  18. Environmental stresses and strains in an extreme situation: the repair of electrometallurgy furnaces.

    Science.gov (United States)

    Chaurel, C; Mercier-Gallay, M; Stoklov, M; Romazini, S; Perdrix, A

    1993-01-01

    Whenever continuous casting furnace breaks down, the emergency intervention necessary to repair it has to be carried out under exceptional environmental conditions caused mainly by heat, as the furnace must be stopped for the shortest possible time. In this study, we aimed to evaluate the stresses and strains to which boilermakers are subjected during the replacement of an electrode element of a 20 MW furnace. The thermal stress was evaluated by the wet bulb globe temperature (WBGT) index. CO2 was measured continuously at the furnace periphery and sporadically in the center of the furnace using an electrochemical method, while CO was also measured in both areas, using Dräger tubes. Dusts were sampled by a CPM3 (Andersen particle fractionating sampler) and a CIP10 (personal sampler). The strain was evaluated by continuous ECG recording with an Aclan IFC 85, breathing performance was assessed with an HI 298 microspirometer, and blood oxygen saturation was evaluated using a Biox oximeter. Thermal stresses are extreme: WBGT was 55 degrees C in the furnace center and 34 degrees C in the furnace periphery. In spite of the ventilation, the reduction in heat during the 6 h of the intervention was negligible and did not provide sufficient cooling. The analysis of gases and dusts were of minor interest, although the mean CO level at the furnace periphery was 40 ppm, with a peak level of 140 ppm in furnace center. CO2 and SO2 levels did not exceed TLV-TWA and TLV-Stel values.(ABSTRACT TRUNCATED AT 250 WORDS)

  19. Atomic resolution images of graphite in air

    Energy Technology Data Exchange (ETDEWEB)

    Grigg, D.A.; Shedd, G.M.; Griffis, D.; Russell, P.E.

    1988-12-01

    One sample used for proof of operation for atomic resolution in STM is highly oriented pyrolytic graphite (HOPG). This sample has been imaged with many different STM`s obtaining similar results. Atomic resolution images of HOPG have now been obtained using an STM designed and built at the Precision Engineering Center. This paper discusses the theoretical predictions and experimental results obtained in imaging of HOPG.

  20. Orgin of Slag from Early Medieval Age Furnaces in Nitra

    Directory of Open Access Journals (Sweden)

    Julius Dekan

    2005-01-01

    Full Text Available Two types of archaeological artefacts from remains of Early Medieval Age furnaces excavated in Nitra are analysed. They are supposed to originate from slag of glass and iron production. Employing Mossbauer spectrometry, iron crystallographic sites are identified and compared. In all samples, Fe2+ and Fe3+ structural positions were revealed. Some of the archeological artefacts including those that were supposed to originate from glass production show a presence of metallic iron and/or magnetic oxides. Based on the results of Mossbauer effect measurements performed at room temperature as well as 77 K (liquid nitrogen temperature analytical evidence is provided that the iron sites identified are not as those usually encountered in glasses. Consequently, a conclusion is proposed that neither of the investigated furnaces was used for glass production.

  1. Annealing furnace for III-V semiconductor devices

    Science.gov (United States)

    O'Connor, J. M.; Hier, H. S.; Ketchum, R. M.

    1986-02-01

    A furnace for annealing ion implantation damage in III-V semiconductors has been built and tested. Designed for research applications, the furnace can accommodate odd shapes of material up to 2 in. in diameter. Samples are loaded onto a novel cantilevered support and are not moved during the annealing operation, facilitating proximity annealing techniques. Both chambers of this dual chambered system are O-ring sealed for added safety during annealing in an arsine gas ambient. Electron mobilities between 4400 and 4600 cm2/V s at 300 K are routinely measured for 2×1017 cm-3 gallium arsenide material annealed in this sytem. The system has been used to anneal indium phosphide as well as gallium arsenide wafers.

  2. Control of the Gas Flow in an Industrial Directional Solidification Furnace for Production of High Purity Multicrystalline Silicon Ingots

    Directory of Open Access Journals (Sweden)

    Lijun Liu

    2015-01-01

    Full Text Available A crucible cover was designed as gas guidance to control the gas flow in an industrial directional solidification furnace for producing high purity multicrystalline silicon. Three cover designs were compared to investigate their effect on impurity transport in the furnace and contamination of the silicon melt. Global simulations of coupled oxygen (O and carbon (C transport were carried out to predict the SiO and CO gases in the furnace as well as the O and C distributions in the silicon melt. Cases with and without chemical reaction on the cover surfaces were investigated. It was found that the cover design has little effect on the O concentration in the silicon melt; however, it significantly influences CO gas transport in the furnace chamber and C contamination in the melt. For covers made of metal or with a coating on their surfaces, an optimal cover design can produce a silicon melt free of C contamination. Even for a graphite cover without a coating, the carbon concentration in the silicon melt can be reduced by one order of magnitude. The simulation results demonstrate a method to control the contamination of C impurities in an industrial directional solidification furnace by crucible cover design.

  3. Bromine intercalated graphite for lightweight composite conductors

    KAUST Repository

    Amassian, Aram

    2017-07-20

    A method of fabricating a bromine-graphite/metal composite includes intercalating bromine within layers of graphite via liquid-phase bromination to create brominated-graphite and consolidating the brominated-graphite with a metal nanopowder via a mechanical pressing operation to generate a bromine-graphite/metal composite material.

  4. Cast construction elements for heat treatment furnaces

    Directory of Open Access Journals (Sweden)

    B. Piekarski

    2011-07-01

    Full Text Available The study presents sketches and photos of the cast creep-resistant components used in various types of heat treatment furnaces. The shape of the elements results from the type of the operation carried out in the furnace, while dimensions are adjusted to the size of the furnace working chamber. The castings are mainly made from the high-alloyed, austenitic chromium-nickel or nickel-chromium steel, selecting the grade in accordance with the furnace operating conditions described by the rated temperature, the type and parameters of the applied operating atmosphere, and the charge weight. Typical examples in this family of construction elements are: crucibles, roller tracks, radiant tubes and guides. The majority of castings are produced in sand moulds.

  5. Blast furnace supervision and control system

    Energy Technology Data Exchange (ETDEWEB)

    Remorino, M.; Lingiardi, O.; Zecchi, M. [Siderar S.A.I.C./Ingdesi, San Nicolas (Argentina)

    1997-12-31

    On December 1992, a group of companies headed by Techint, took over Somisa, the state-owned integrated steel plant located at San Nicolas, Province of Buenos Aires, Argentina, culminating an ambitious government privatization scheme. The blast furnace 2 went into a full reconstruction and relining in January 1995. After a 140 MU$ investment the new blast furnace 2 was started in September 1995. After more than one year of operation of the blast furnace the system has proven itself useful and reliable. The main reasons for the success of the system are: same use interface for all blast furnace areas -- operation, process, maintenance and management, (full horizontal and vertical integration); and full accessibility to all information and process tools though some restrictions apply to field commands (people empowerment). The paper describes the central system.

  6. Multiple hearth furnace for reducing iron oxide

    Energy Technology Data Exchange (ETDEWEB)

    Brandon, Mark M [Charlotte, NC; True, Bradford G [Charlotte, NC

    2012-03-13

    A multiple moving hearth furnace (10) having a furnace housing (11) with at least two moving hearths (20) positioned laterally within the furnace housing, the hearths moving in opposite directions and each moving hearth (20) capable of being charged with at least one layer of iron oxide and carbon bearing material at one end, and being capable of discharging reduced material at the other end. A heat insulating partition (92) is positioned between adjacent moving hearths of at least portions of the conversion zones (13), and is capable of communicating gases between the atmospheres of the conversion zones of adjacent moving hearths. A drying/preheat zone (12), a conversion zone (13), and optionally a cooling zone (15) are sequentially positioned along each moving hearth (30) in the furnace housing (11).

  7. Chamberless residential warm air furnace design

    Energy Technology Data Exchange (ETDEWEB)

    Godfree, J. [Product Design consultant, Pugwash (Canada)

    1996-07-01

    This brief paper is an introduction to the concept of designing residential warm air furnaces without combustion chambers. This is possible since some small burners do not require the thermal support of a combustion chamber to complete the combustion process.

  8. METALLURGICAL ADVANTAGES OF ROTATION TILTING FURNACES

    Directory of Open Access Journals (Sweden)

    S. L. Rovin

    2010-01-01

    Full Text Available It is shown that introduction of rotary tilting furnaces can be a basis for considerable resources saving, lowering of power inputs, reduction of products cost for Byelorussian machine-building enterprises.

  9. Modular Distributed Concentrator for Solar Furnace Project

    Data.gov (United States)

    National Aeronautics and Space Administration — This research proposes to develop a lightweight approach to achieving the high concentrations of solar energy needed for a solar furnace achieving temperatures of...

  10. Cluster Ion Implantation in Graphite and Diamond

    DEFF Research Database (Denmark)

    Popok, Vladimir

    2014-01-01

    Cluster ion beam technique is a versatile tool which can be used for controllable formation of nanosize objects as well as modification and processing of surfaces and shallow layers on an atomic scale. The current paper present an overview and analysis of data obtained on a few sets of graphite a...... implantation. Implantation of cobalt and argon clusters into two different allotropic forms of carbon, namely, graphite and diamond is analysed and compared in order to approach universal theory of cluster stopping in matter.......Cluster ion beam technique is a versatile tool which can be used for controllable formation of nanosize objects as well as modification and processing of surfaces and shallow layers on an atomic scale. The current paper present an overview and analysis of data obtained on a few sets of graphite...... and diamond samples implanted by keV-energy size-selected cobalt and argon clusters. One of the emphases is put on pinning of metal clusters on graphite with a possibility of following selective etching of graphene layers. The other topic of concern is related to the development of scaling law for cluster...

  11. Paired Straight Hearth Furnace - Transformational Ironmaking Process

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Wei-Kao [McMaster Univ., Hamilton, ON (Canada); Debski, Paul [Andritz Metals Inc.,Canonsburg, PA (United States)

    2014-11-19

    The U. S. steel industry has reduced its energy intensity per ton of steel shipped by 33% since 1990. However, further significant gains in energy efficiency will require the development of new, transformational iron and steelmaking processes. The Paired Straight Hearth Furnace (PSH) process is an emerging alternative high productivity, direct reduced iron (DRI) technology that may achieve very low fuel rates and has the potential to replace blast furnace ironmaking. The PSH furnace can operate independently or may be coupled with other melting technologies to produce liquid hot metal that is both similar to blast furnace iron and suitable as a feedstock for basic oxygen steelmaking furnaces. The PSH process uses non-metallurgical coal as a reductant to convert iron oxides such as iron ore and steelmaking by-product oxides to DRI pellets. In this process, a multi-layer, nominally 120mm tall bed of composite “green balls” made from oxide, coal and binder is built up and contained within a moving refractory hearth. The pellet bed absorbs radiant heat energy during exposure to the high temperature interior refractory surfaces of the PSH while generating a strongly reducing gas atmosphere in the bed that yields a highly metalized DRI product. The PSH concept has been well tested in static hearth experiments. A moving bed design is being developed. The process developers believe that if successful, the PSH process has the potential to replace blast furnaces and coke ovens at a fraction of the operating and capital cost while using about 30% less energy relative to current blast furnace technology. DRI output could also feed electric arc furnaces (EAFs) by displacing a portion of the scrap charge.

  12. Waste and dust utilisation in shaft furnaces

    OpenAIRE

    Senk, D.; Babich, A.; Gudenau, H. W.

    2005-01-01

    Wastes and dusts from steel industry, non-ferrous metallurgy and other branches can be utilized e.g. in agglomeration processes (sintering, pelletizing or briquetting) and by injection into shaft furnaces. This paper deals with the second way. Combustion and reduction behaviour of iron- and carbon-rich metallurgical dusts and sludges containing lead, zinc and alkali as well as other wastes with and without pulverized coal (PC) has been studied when injecting into shaft furnaces. Following sha...

  13. Solar Convective Furnace for Metals Processing

    Science.gov (United States)

    Patidar, Deepesh; Tiwari, Sheetanshu; Sharma, Piyush; Pardeshi, Ravindra; Chandra, Laltu; Shekhar, Rajiv

    2015-11-01

    Metals processing operations, primarily soaking, heat treatment, and melting of metals are energy-intensive processes using fossil fuels, either directly or indirectly as electricity, to operate furnaces at high temperatures. Use of concentrated solar energy as a source of heat could be a viable "green" option for industrial heat treatment furnaces. This paper introduces the concept of a solar convective furnace which utilizes hot air generated by an open volumetric air receiver (OVAR)-based solar tower technology. The potential for heating air above 1000°C exists. Air temperatures of 700°C have already been achieved in a 1.5-MWe volumetric air receiver demonstration plant. Efforts to retrofit an industrial aluminium soaking furnace for integration with a solar tower system are briefly described. The design and performance of an OVAR has been discussed. A strategy for designing a 1/15th-scale model of an industrial aluminium soaking furnace has been presented. Preliminary flow and thermal simulation results suggest the presence of recirculating flow in existing furnaces that could possibly result in non-uniform heating of the slabs. The multifarious uses of concentrated solar energy, for example in smelting, metals processing, and even fuel production, should enable it to overcome its cost disadvantage with respect to solar photovoltaics.

  14. Information modeling system for blast furnace control

    Science.gov (United States)

    Spirin, N. A.; Gileva, L. Y.; Lavrov, V. V.

    2016-09-01

    Modern Iron & Steel Works as a rule are equipped with powerful distributed control systems (DCS) and databases. Implementation of DSC system solves the problem of storage, control, protection, entry, editing and retrieving of information as well as generation of required reporting data. The most advanced and promising approach is to use decision support information technologies based on a complex of mathematical models. The model decision support system for control of blast furnace smelting is designed and operated. The basis of the model system is a complex of mathematical models created using the principle of natural mathematical modeling. This principle provides for construction of mathematical models of two levels. The first level model is a basic state model which makes it possible to assess the vector of system parameters using field data and blast furnace operation results. It is also used to calculate the adjustment (adaptation) coefficients of the predictive block of the system. The second-level model is a predictive model designed to assess the design parameters of the blast furnace process when there are changes in melting conditions relative to its current state. Tasks for which software is developed are described. Characteristics of the main subsystems of the blast furnace process as an object of modeling and control - thermal state of the furnace, blast, gas dynamic and slag conditions of blast furnace smelting - are presented.

  15. Dynamic Mechanical Properties of Bio-Polymer Graphite Thin Films

    Science.gov (United States)

    Saddam Kamarudin, M.; Rus, Anika Zafiah M.; Munirah Abdullah, Nur; Abdullah, M. F. L.

    2017-08-01

    Waste cooking oil is used as the main substances in producing graphite biopolymer thin films. Biopolymer is produce from the reaction of bio-monomer and cross linker with the ratio of 2:1 and addition of graphite with an increment of 2% through a slip casting method. The morphological surface properties of the samples are observed by using Scanning Electron Microscope (SEM). It is shown that the graphite particle is well mixed and homogenously dispersed in biopolymer matrix. Meanwhile, the mechanical response of materials by monitoring the change in the material properties in terms of frequency and temperature of the samples were determined using Dynamic Mechanical Analysis (DMA). The calculated cross-linked density of biopolymer composites revealed the increment of graphite particle loading at 8% gives highest results with 260.012 x 103 M/m3.

  16. Heat exchanger using graphite foam

    Science.gov (United States)

    Campagna, Michael Joseph; Callas, James John

    2012-09-25

    A heat exchanger is disclosed. The heat exchanger may have an inlet configured to receive a first fluid and an outlet configured to discharge the first fluid. The heat exchanger may further have at least one passageway configured to conduct the first fluid from the inlet to the outlet. The at least one passageway may be composed of a graphite foam and a layer of graphite material on the exterior of the graphite foam. The layer of graphite material may form at least a partial barrier between the first fluid and a second fluid external to the at least one passageway.

  17. Dual functions of TiC nanoparticles on tribological performance of Al/graphite composites

    Science.gov (United States)

    Fallahdoost, Hamid; Nouri, Alireza; Azimi, Amin

    2016-06-01

    In this study, the effect of TiC nanoparticles as a reinforcement on the mechanical and tribological properties of Aluminum-based self lubricating composite was investigated. The microstructure, relative density, hardness, and tribological properties of Al/graphite and Al/TiC/graphite composites were examined as a function of graphite content. The tribo-surfaces of the samples were analyzed using SEM and EDS elemental mapping. The results indicated that the addition of TiC nanoparticles not only decreased the wear rate and coefficient of friction of the composites, but also facilitated the formation of a stable graphite layer at longer sliding distances and high sliding velocities by forming a durable graphite/TiC composite on the tribo-surface. Therefore, the stability of graphite layer can be considered as a possible cause for decrease in wear rate of the Al/TiC/graphite composite.

  18. A Comparison Study of the Oxygen-Rich Side Blow Furnace and the Oxygen-Rich Bottom Blow Furnace for Liquid High Lead Slag Reduction

    Science.gov (United States)

    Chen, Lin; Hao, Zhandong; Yang, Tianzu; Liu, Weifeng; Zhang, Duchao; Zhang, Li; Bin, Shu; Bin, Wanda

    2015-05-01

    This work investigates the characteristics of the oxygen-rich side blow furnace (OSBF) and the oxygen-rich bottom blow furnace (OBBF) as the reductive smelting reactor for molten high lead slag. The slags were collected from different sampling points of these furnaces during a regular high lead slag reduction process and analyzed. It is disclosed that lead content of the melt in the OSBF shows dramatic fluctuations, while melt from different sampling points of the furnace behave similarly, exhibiting the characteristics of batch reactor. An obvious axial lead content gradient is detected in the OBBF, showing the characteristics of a plug flow reactor. The industrial performances of these furnaces are also compared. The results indicate that 1.38% higher lead recovery can be achieved by using the OSBF instead of the OBBF. Unit energy consumptions of the OBBF-OSBF and OBBF-OBBF processes can be reduced to 230 kgce/ t crude lead, which is 70 kgce/ t crude lead less than that of the tradition Shuikoushan (SKS) process.

  19. 3-D Analysis of Graphite Nodules in Ductile Cast Iron Using FIB-SEM

    DEFF Research Database (Denmark)

    D'Angelo, Luca; Jespersen, Freja N.; MacDonald, A. Nicole

    Ductile cast iron samples were analysed in a Focused Ion Beam Scanning Electron Microscope, FIB-SEM. The focussed ion beam was used to carefully remove layers of the graphite nodules to reveal internal structures in the nodules. The sample preparation and milling procedure for sectioning graphite...... inside the nodules, their orientation in relation to the graphite and the chemistry of the inclusions is analysed and described. Formation of the structures during solidification and subsequent cooling to room temperature is discussed....

  20. Characterization of a Mono-Ellipsoidal Imaging Furnace

    Energy Technology Data Exchange (ETDEWEB)

    Guesdon, C.; Alxneit, I.; Tschudi, H.R.; Wuillemin, D.; Brunner, Y.; Winkel, L.; Sturzenegger, M.

    2004-03-01

    An imaging furnace was built and tested for investigating chemical reactions that involve melts and the release of condensable gases. A key feature is the sample stage with a water-cooled sample support to avoid reaction of the sample with crucible material. A built-in hammer allows for freezing the high-temperature composition of the sample and a glass dome above the sample allows for experiments under defined atmospheres. Measured peak flux densities on samples with a diameter of 5 mm clearly exceed 500 Wcm{sub -2} producing sample temperatures of at least 2500 K. Cold experiments with a smoke source at the place of the sample as well as decomposition experiments with chalcocite (Cu{sub 2}S) proved that an appropriate gas flow through the dome keeps the dome free of condensates. (author)

  1. APPLICATION OF MODIFYING ALLOYING ALLOY CONTAINING NANOSIZED POWDERS OF ACTIVE ELEMENTS IN PRODUCTION OF HIGH-STRENGTH CAST IRON WITH GLOBULAR GRAPHITE

    Directory of Open Access Journals (Sweden)

    A. S. Kalinichenko

    2015-01-01

    Full Text Available Scientific and practical interest is the application of alloying alloy-modifiers for secondary treatment of high-strength cast iron to stabilize the process of spheroidization graphite and achieving higher physical-mechanical properties of castings. The peculiarity of the high-strength cast irons manufacturing technology is their tendency to supercooling during solidification in the mold. This leads to the formation of shrinkage defects and structurally free cementite, especially in thin-walled sections of the finished castings. To minimize these effects in foundry practice during production of ductile iron the secondary inoculation is widely used. In this regard, the question of the choice of the additives with effective impact not only on the graphitization process but also on the formation of the metallic base of ductile iron is relevant. The aim of the present work is to study the peculiarities of structure formation in cast iron with nodular graphite when alloying alloy-modifier based on tin with additions of nanoparticles of titanium carbide, yttrium oxide and graphite nano-pipes is used for secondary treatment. Melting of iron in laboratory conditions was performed in crucible induction furnace IST-006 with an acid lining held. Spheroidizing treatment of melt was realized with magnesium containing alloying alloy FeSiMg7 by means of ladle method. Secondary treatment of high strength cast iron was carried out by addition of alloying alloy-modifier in an amount of 0.1% to the bottom of the pouring ladle. Cast samples for chemical composition analysis, study of microstructure, technological and mechanical properties of the resultant alloy were made. Studies have shown that the secondary treatment of high strength cast iron with developed modifier-alloying alloy results in formation of the perlite metallic base due to the tin impact and nodular graphite with regular shape under the influence of titanium carbide, yttrium oxide and graphite nano

  2. Synthesis of carbon nanotubes by laser ablation in graphite substrate of industrial arc electrodes

    Science.gov (United States)

    Guerrero, A.; Puerta, J.; Gomez, F.; Blanco, F.

    2008-10-01

    In this work, an inexpensive and simple technique for the synthesis of carbon nanotubes (CNTs) by using graphite as the target for IR laser radiation is presented. This graphite material is obtained from the recycled graphite electrode core of an electric arc furnace. The experiment was carried out in a reaction chamber in an argon atmosphere at a low pressure. For laser ablation, a Lumonics TEA CO2 laser beam (7 J; 0.05-50 μs pulse length) was used in multimode operation. Products were collected on free mica sheets. The substrates were characterized by scanning electron microscopy (SEM) and the products were characterized (collected as powder) by transmission electron microscopy (TEM). They showed significant amounts of high-quality dense filaments (CNTs) that were morphologically not aligned.

  3. Erection of duct-like graphitic carbon nitride with enhanced photocatalytic activity for ACB photodegradation

    Science.gov (United States)

    Muhmood, Tahir; Xia, Mingzhu; Lei, Wu; Wang, Fengyun

    2018-02-01

    Novel duct graphitic carbon nitride (DCN) was successfully prepared using the temperature control method in a quartz tube furnace from commercially available melamine and evaluated against the photo-degradation of latent organic pollutants, acarbose (ACB). These prepared materials were characterized by UV–Vis spectroscopy, Fourier transform infrared spectra, x-ray photoelectron spectroscopy, x-ray diffraction, transmission electron microscopy and scanning electron microscopy. The characterization results indicated that the synthesized material was in the form of a duct-like structure and has greater adsorption capacity and photocatalytic ability as compared to traditionally synthesized graphitic carbon nitride materials. The DCN split theACB completely into many intermediates, which were depicted in the HPLC-MS spectrum for knowing the acarbose photo-degrdation pathway. The duct-like morphology of graphitic carbon nitride has improved properties, such as increasing the surface area and decelerating the e ‑/h + recombination, which increase the light absorbance ability with enhanced photoactivity.

  4. Characterization of nuclear graphite elastic properties using laser ultrasonic methods

    Energy Technology Data Exchange (ETDEWEB)

    Zeng, Fan W [Johns Hopkins University; Han, Karen [Johns Hopkins University; Olasov, Lauren R [Johns Hopkins University; Gallego, Nidia C [ORNL; Contescu, Cristian I [ORNL; Spicer, James B [Johns Hopkins University

    2015-01-01

    Laser ultrasonic methods have been used to characterize the elastic behaviors of commercially-available and legacy nuclear graphites. Since ultrasonic techniques are sensitive to various aspects of graphite microstructure including preferred grain orientation, microcrack orientation and porosity, laser ultrasonics is a candidate technique for monitoring graphite degradation and structural integrity in environments expected in high-temperature, gas-cooled nuclear reactors. Aspects of materials texture can be assessed by studying ultrasonic wavespeeds as a function of propagation direction and polarization. Shear wave birefringence measurements, in particular, can be used to evaluate elastic anisotropy. In this work, laser ultrasonic measurements of graphite moduli have been made to provide insight into the relationship between the microstructures and the macroscopic stiffnesses of these materials. In particular, laser ultrasonic measurements have been made using laser line sources to produce shear waves with specific polarizations. By varying the line orientation relative to the sample, shear wave birefringence measurements have been recorded. Results from shear wave birefringence measurements show that an isostatically molded graphite, such as PCIB, behaves isotropically, while an extruded graphite, such as H-451, displays significant ultrasonic texture. Graphites have complicated microstructures that depend on the manufacturing processes used, and ultrasonic texture in these materials could originate from grain orientation and preferred microcrack alignment. Effects on material isotropy due to service related microstructural changes are possible and the ultimate aim of this work is to determine the degree to which these changes can be assessed nondestructively using laser ultrasonics measurements

  5. ADDITION OF ELECTRIC ARC FURNACE DUST IN HOT METAL

    Directory of Open Access Journals (Sweden)

    Felipe Fardin Grillo

    2013-03-01

    Full Text Available This research aims to study the process of incorporation of the mass in final hot metal and volatilization mass contained in the electric arc furnace dust (EAFD, by addition in hot metal at a temperature of 1,400°C; 1,450°C and 1,500°C altering experimental conditions such as the percentage of EAFD to be added and the percentage of silicon in hot metal. Previously, the EAFD was characterized using techniques of chemical analysis and size analysis. After characterization, the EAFD to be added to the hot metal was agglomerated in the form of briquettes. The achievement of fusion experiments in laboratory scale was placed in a vertical tubular furnace with temperature control. A flow of inert gas (argon was maintained inside the furnace during the experiments. The result of the sample EAFD volatilized shows that there is an increase in the zinc concentration when compared with the concentration of zinc present in EAFD “as received”.

  6. Study of ultraviolet-visible light absorbance of exfoliated graphite forms

    Directory of Open Access Journals (Sweden)

    S. Uran

    2017-03-01

    Full Text Available Despite the fact that there have been many studies of graphite exfoliation, none really addresses the issue of starting form of graphite. To address this issue various graphite forms (solid, powder and sooth and graphite oxide (powder are exfoliated in acetonitrile and studied via ultraviolet-visible (UV-Vis spectroscopy. In different graphite forms two major absorbance peaks are observed at 223 nm and 273 nm corresponding to graphene oxide and graphene dispersions, respectively. The intensity change of the peaks refers to the layer number change. The intensity ratios of these peaks give information about the concentration of the exfoliation products. We observed that graphite oxide sample has the thinnest graphene dispersions among the compared samples, whereas graphite rod has the thickest. It appears that few layer graphene oxide dispersions exist more in graphite sooth and graphite oxide samples. Graphite oxide UV-Vis spectrum reveals two new absorbance peaks at 312 nm and 361 nm in addition to the graphene oxide and graphene dispersion peaks. To our knowledge these peaks were not observed before. We think that these new peaks are formed due to conjugated polyenes that affect π → π* plasmon peak.

  7. Study of ultraviolet-visible light absorbance of exfoliated graphite forms

    Science.gov (United States)

    Uran, S.; Alhani, A.; Silva, C.

    2017-03-01

    Despite the fact that there have been many studies of graphite exfoliation, none really addresses the issue of starting form of graphite. To address this issue various graphite forms (solid, powder and sooth) and graphite oxide (powder) are exfoliated in acetonitrile and studied via ultraviolet-visible (UV-Vis) spectroscopy. In different graphite forms two major absorbance peaks are observed at 223 nm and 273 nm corresponding to graphene oxide and graphene dispersions, respectively. The intensity change of the peaks refers to the layer number change. The intensity ratios of these peaks give information about the concentration of the exfoliation products. We observed that graphite oxide sample has the thinnest graphene dispersions among the compared samples, whereas graphite rod has the thickest. It appears that few layer graphene oxide dispersions exist more in graphite sooth and graphite oxide samples. Graphite oxide UV-Vis spectrum reveals two new absorbance peaks at 312 nm and 361 nm in addition to the graphene oxide and graphene dispersion peaks. To our knowledge these peaks were not observed before. We think that these new peaks are formed due to conjugated polyenes that affect π → π* plasmon peak.

  8. Planar lighting from optimized graphite papers made of graphite oxide

    Science.gov (United States)

    Tan, Ziqi; Xu, Huailiang; Zhou, Bucun; Qi, Zeming; Qu, Yan; Zhu, Yanwu

    2017-05-01

    We report the preparation of large-area graphite papers with thicknesses from 100 μm to more than 1 mm, by the reduction and graphitization of graphite oxide at elevated temperatures. The papers can be produced on a size of 20 × 20 cm2 and have a low mass density. X-ray diffraction and Raman characterization show that the stacking of graphitic layers in the papers follows the Bernal stacking, and X-ray photoelectron spectroscopy indicates a carbon purity of above 98 at. % in the papers. The graphite papers have an electrical conductivity of 2533-4996 S/m and a thermal conductivity of 42-149 W/mK, depending on the thickness. When a power input of above 10 W is applied on the paper with a thickness of 98 μm, incandescence is observed, corresponding to a temperature of higher than 1000 °C, which is increased with the input power.

  9. Graphite in Science and Nuclear Technique

    OpenAIRE

    Zhmurikov, E. I.; Bubnenkov, I. A.; Dremov, V. V.; Samarin, S. I.; Pokrovsky, A. S.; Harkov, D. V.

    2013-01-01

    The monograph is devoted to the application of graphite and graphite composites in science and technology. The structure and electrical properties, the technological aspects of production of high-strength synthetic graphites, the dynamics of the graphite destruction, traditionally used in the nuclear industry are discussed. It is focuses on the characteristics of graphitization and properties of graphite composites based on carbon isotope 13C. The book is based, generally, on the original res...

  10. Interfacial reaction between zirconium alloy and graphite mold/yttrium oxide ceramic mold

    Directory of Open Access Journals (Sweden)

    Xie Huasheng

    2014-03-01

    Full Text Available Zirconium alloys are active in the molten state and tend to react with the mold during casting. The casting technology of zirconium is not yet well established; especially in selecting the mold materials, which are difficult to determine. In the present work, the interfacial reactions between zirconium casting and casting mold were studied. The zirconium alloy was melted in a vacuum arc skull furnace and then cast into the graphite mold and ceramic mold, respectively. The zirconium casting samples were characterized using SEM, EDS and XRD with an emphasis on the chemical diffusion of elements. A reaction layer was observed at the casting surface. Chemical analysis shows that chemical elements C, O and Y from the mold are diffused into the molten zirconium, and new phases, such as ZrC, Zr3O, YO1.335 and Y6ZrO11, are formed at the surface. In addition, an end product of zirconium valve cast in a yttria mold has a compact structure and good surface quality.

  11. Graphite fluoride fibers and their applications in the space industry

    Science.gov (United States)

    Hung, Ching-Chen; Long, Martin; Dever, Therese

    1990-01-01

    Characterization and potential space applications of graphite fluoride fibers from commercially available graphitized carbon fibers are presented. Graphite fluoride fibers with fluorine to carbon ratios of 0.65 and 0.68 were found to have electrical resistivity values of 10(exp 4) and 10(exp 11) Ohms-cm, respectively, and thermal conductivity values of 24 and 5 W/m-K, respectively. At this fluorine content range, the fibers have tensile strength of 0.25 + or - 0.10 GPa (36 + or - 14 ksi), Young's modulus of 170 + or - 30 GPa (25 + or - 5 Msi). The coefficient of thermal expansion value of a sample with fluorine to carbon ratio of 0.61 was found to be 7 ppm/C. These properties change and approach the graphite value as the fluorine content approach 0. Electrically insulative graphite fluoride fiber is at least five times more thermally conductive than fiberglass. Therefore, it can be used as a heat sinking printed circuit board material for low temperature, long life power electronics in spacecraft. Also, partially fluorinated fiber with tailor-made physical properties to meet the requirements of certain engineering design can be produced. For example, a partially fluorinated fiber could have a predetermined CTE value in -1.5 to 7 ppm/C range and would be suitable for use in solar concentrators in solar dynamic power systems. It could also have a predetermined electrical resistivity value suitable for use as a low observable material. Experimental data indicate that slightly fluorinated graphite fibers are more durable in the atomic oxygen environment than pristine graphite. Therefore, fluorination of graphite used in the construction of spacecraft that would be exposed to the low Earth orbit atomic oxygen may protect defect sites in atomic oxygen protective coatings and therefore decrease the rate of degradation of graphite.

  12. Thermal Treatment of Solid Wastes Using the Electric Arc Furnace

    Energy Technology Data Exchange (ETDEWEB)

    O' Connor, W.K.; Turner, P.C.

    1999-09-01

    A thermal waste treatment facility has been developed at the Albany Research Center (ARC) over the past seven years to process a wide range of heterogeneous mixed wastes, on a scale of 227 to 907 kg/h (500 to 2,000 lb/h). The current system includes a continuous feed system, a 3-phase AC, 0.8 MW graphite electrode arc furnace, and a dedicated air pollution control system (APCS) which includes a close-coupled thermal oxidizer, spray cooler, baghouse, and wet scrubber. The versatility of the complete system has been demonstrated during 5 continuous melting campaigns, ranging from 11 to 25 mt (12 to 28 st) of treated wastes per campaign, which were conducted on waste materials such as (a) municipal incinerator ash, (b) simulated low-level radioactive, high combustible-bearing mixed wastes, (c) simulated low-level radioactive liquid tank wastes, (d) heavy metal contaminated soils, and (e) organic-contaminated dredging spoils. In all cases, the glass or slag products readily passed the U.S. Environmental Protection Agency (EPA) Toxicity Characteristic Leachability Program (TCLP) test. Additional studies are currently under way on electric utility wastes, steel and aluminum industry wastes, as well as zinc smelter residues. Thermal treatment of these solid waste streams is intended to produce a metallic product along with nonhazardous glass or slag products.

  13. REFRACTORY COATING FOR GRAPHITE MOLDS

    Science.gov (United States)

    Stoddard, S.D.

    1958-06-24

    Refractory coating for graphite molds used in the casting of uranium is described. The coating is an alumino-silicate refractory composition which may be used as a mold surface in solid form or as a coating applied to the graphite mold. The composition consists of a mixture of ball clay, kaolin, alumina cement, alumina, water, sodium silicate, and sodium carbonate.

  14. Cryotribology of diamond and graphite

    Energy Technology Data Exchange (ETDEWEB)

    Iwasa, Yukikazu; Ashaboglu, A.F.; Rabinowicz, E.R. [Francis Bitter Magnet Lab., Cambridge, MA (United States)

    1996-12-31

    An experimental study was carried out on the tribological behavior of materials of interest in cryogenic applications, focusing on diamond and graphite. Both natural diamond (referred in the text as diamond) and chemical-vapor-deposition (CVD) diamond (CVD-diamond) were used. The experiment was carried out using a pin-on-disk tribometer capable of operating at cryogenic temperatures, from 4.2 to 293 K. Two basic scenarios of testing were used: (1) frictional coefficient ({mu}) vs velocity (v) characteristics at constant temperatures; (2) {mu} vs temperature (T) behavior at fixed sliding speeds. For diamond/CVD-diamond, graphite/CVD-diamond, stainless steel/CVD-diamond pairs, {mu}`s are virtually velocity independent. For each of diamond/graphite, alumina/graphite, and graphite/graphite pairs, the {partial_derivative}{mu}/{partial_derivative}v characteristic is favorable, i.e., positive. For diamond/CVD-diamond and graphite/CVD-diamond pairs, {mu}`s are nearly temperature independent between in the range 77 - 293 K. Each {mu} vs T plot for pin materials sliding on graphite disks has a peak at a temperature in the range 100 - 200 K.

  15. Pristine graphite oxide.

    Science.gov (United States)

    Dimiev, Ayrat; Kosynkin, Dmitry V; Alemany, Lawrence B; Chaguine, Pavel; Tour, James M

    2012-02-08

    Graphite oxide (GO) is a lamellar substance with an ambiguous structure due to material complexity. Recently published GO-related studies employ only one out of several existing models to interpret the experimental data. Because the models are different, this leads to confusion in understanding the nature of the observed phenomena. Lessening the structural ambiguity would lead to further developments in functionalization and use of GO. Here, we show that the structure and properties of GO depend significantly on the quenching and purification procedures, rather than, as is commonly thought, on the type of graphite used or oxidation protocol. We introduce a new purification protocol that produces a product that we refer to as pristine GO (pGO) in contrast to the commonly known material that we will refer to as conventional GO (cGO). We explain the differences between pGO and cGO by transformations caused by reaction with water. We produce ultraviolet-visible spectroscopic, Fourier transform infrared spectroscopic, solid-state nuclear magnetic resonance spectroscopic, thermogravimetric, and scanning electron microscopic analytical evidence for the structure of pGO. This work provides a new explanation for the acidity of GO solutions and allows us to add critical details to existing GO models.

  16. Baseline Graphite Characterization: First Billet

    Energy Technology Data Exchange (ETDEWEB)

    Mark C. Carroll; Joe Lords; David Rohrbaugh

    2010-09-01

    The Next Generation Nuclear Plant Project Graphite Research and Development program is currently establishing the safe operating envelope of graphite core components for a very high temperature reactor design. To meet this goal, the program is generating the extensive amount of quantitative data necessary for predicting the behavior and operating performance of the available nuclear graphite grades. In order determine the in-service behavior of the graphite for the latest proposed designs, two main programs are underway. The first, the Advanced Graphite Creep (AGC) program, is a set of experiments that are designed to evaluate the irradiated properties and behavior of nuclear grade graphite over a large spectrum of temperatures, neutron fluences, and compressive loads. Despite the aggressive experimental matrix that comprises the set of AGC test runs, a limited amount of data can be generated based upon the availability of space within the Advanced Test Reactor and the geometric constraints placed on the AGC specimens that will be inserted. In order to supplement the AGC data set, the Baseline Graphite Characterization program will endeavor to provide supplemental data that will characterize the inherent property variability in nuclear-grade graphite without the testing constraints of the AGC program. This variability in properties is a natural artifact of graphite due to the geologic raw materials that are utilized in its production. This variability will be quantified not only within a single billet of as-produced graphite, but also from billets within a single lot, billets from different lots of the same grade, and across different billets of the numerous grades of nuclear graphite that are presently available. The thorough understanding of this variability will provide added detail to the irradiated property data, and provide a more thorough understanding of the behavior of graphite that will be used in reactor design and licensing. This report covers the

  17. Properties of metal atoms hosted inside graphite's layer lattice

    Science.gov (United States)

    Rahman, F.

    2007-02-01

    Graphite samples containing several different metals have been prepared and their optical, electrical and magnetic properties investigated. It was found that ordinary metals lose their characteristic metallic lustre on incorporation inside graphite and thus their optical reflectivities are greatly reduced. Electrical conduction of graphite is only slightly altered by transition metal hosting and these observations point towards an absence of metal-donated free electron gas in such composite materials. Nanoscale iron oxide particles are easily accommodated inside graphite’s structure through doping with a ferrofluid and again an absence of long range cooperative effects is observed. Iron oxide-containing graphite exhibits strong paramagnetic behaviour and it was used to make cores for high frequency signal transformers.

  18. Modeling and control of a calcination furnace

    OpenAIRE

    Wilson, Øyvind

    2017-01-01

    Calcined anthracite is the primary material used in Søderberg electrode paste, prebaked carbon electrodes, aluminium cathodes, and a variety of other carbon products used in the metallurgical industries. In electrical calcination of anthracite current is passed through the raw material. This heat treats the anthracite, which gets rid of volatile matter and water, and graphitizes the anthracite. The graphitization lower the anthracite's electrical resistivity. The object of the process is...

  19. Industrial and process furnaces principles, design and operation

    CERN Document Server

    Jenkins, Barrie

    2014-01-01

    Furnaces sit at the core of all branches of manufacture and industry, so it is vital that these are designed and operated safely and effi-ciently. This reference provides all of the furnace theory needed to ensure that this can be executed successfully on an industrial scale. Industrial and Process Furnaces: Principles, 2nd Edition provides comprehensive coverage of all aspects of furnace operation and design, including topics essential for process engineers and operators to better understand furnaces. This includes: the combustion process and its control, furnace fuels, efficiency,

  20. Cogeneration from glass furnace waste heat recovery

    Energy Technology Data Exchange (ETDEWEB)

    Hnat, J.G.; Cutting, J.C.; Patten, J.S.

    1982-06-01

    In glass manufacturing 70% of the total energy utilized is consumed in the melting process. Three basic furnaces are in use: regenerative, recuperative, and direct fired design. The present paper focuses on secondary heat recovery from regenerative furnaces. A diagram of a typical regenerative furnace is given. Three recovery bottoming cycles were evaluated as part of a comparative systems analysis: steam Rankine Cycle (SRC), Organic Rankine Cycle (ORC), and pressurized Brayton cycle. Each cycle is defined and schematicized. The net power capabilities of the three different systems are summarized. Cost comparisons and payback period comparisons are made. Organic Rankine cycle provides the best opportunity for cogeneration for all the flue gas mass flow rates considered. With high temperatures, the Brayton cycle has the shortest payback period potential, but site-specific economics need to be considered.

  1. Distribution of trace metals at Hopewell Furnace National Historic Site, Berks and Chester Counties, Pennsylvania

    Science.gov (United States)

    Sloto, Ronald A.; Reif, Andrew G.

    2011-01-01

    Hopewell Furnace, located approximately 50 miles northwest of Philadelphia, was a cold-blast, charcoal iron furnace that operated for 113 years (1771 to 1883). The purpose of this study by the U.S. Geological Survey, in cooperation with the National Park Service, was to determine the distribution of trace metals released to the environment from an historical iron smelter at Hopewell Furnace National Historic Site (NHS). Hopewell Furnace used iron ore from local mines that contained abundant magnetite and accessory sulfide minerals enriched in arsenic, cobalt, copper, and other metals. Ore, slag, cast iron furnace products, soil, groundwater, stream base flow, streambed sediment, and benthic macroinvertebrates were sampled for this study. Soil samples analyzed in the laboratory had concentrations of trace metals low enough to meet Pennsylvania Department of Environmental Protection standards for non-residential use. Groundwater samples from the supply well met U.S. Environmental Protection Agency drinking-water regulations. Concentrations of metals in surface-water base flow at the five stream sampling sites were below continuous concentration criteria for protection of aquatic organisms. Concentrations of metals in sediment at the five stream sites were below probable effects level guidelines for protection of aquatic organisms except for copper at site HF-3. Arsenic, copper, lead, zinc, and possibly cobalt were incorporated into the cast iron produced by Hopewell Furnace. Manganese was concentrated in slag along with iron, nickel, and zinc. The soil near the furnace has elevated concentrations of chromium, copper, iron, lead, and zinc compared to background soil concentrations. Concentrations of toxic elements were not present at concentrations of concern in water, soil, or stream sediments, despite being elevated in ore, slag, and cast iron furnace products. The base-flow surface-water samples indicated good overall quality. The five sampled sites generally had

  2. The mid-infrared biconical reflectance of thin films on highly oriented pyrolytic graphite

    Science.gov (United States)

    Anderson, M. S.

    1991-01-01

    Measurements are reported of the biconical reflectance of pyrolytic graphite in the spectral region between 4000 and 600/cm. The measurements are conducted with an FTIR spctrometer with the beam focused to a 1-mm-diam focal point on the sample surface. The highly oriented pyrolytic graphite has a high biconical reflectance as compared to other graphitic materials and does not cause significant beam scattering.

  3. Measure Guideline. High Efficiency Natural Gas Furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Brand, L. [Partnership for Advanced Residential Retrofit (PARR), Des Plaines, IL (United States); Rose, W. [Partnership for Advanced Residential Retrofit (PARR), Des Plaines, IL (United States)

    2012-10-01

    This measure guideline covers installation of high-efficiency gas furnaces, including: when to install a high-efficiency gas furnace as a retrofit measure; how to identify and address risks; and the steps to be used in the selection and installation process. The guideline is written for Building America practitioners and HVAC contractors and installers. It includes a compilation of information provided by manufacturers, researchers, and the Department of Energy as well as recent research results from the Partnership for Advanced Residential Retrofit (PARR) Building America team.

  4. Measure Guideline: High Efficiency Natural Gas Furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Brand, L.; Rose, W.

    2012-10-01

    This Measure Guideline covers installation of high-efficiency gas furnaces. Topics covered include when to install a high-efficiency gas furnace as a retrofit measure, how to identify and address risks, and the steps to be used in the selection and installation process. The guideline is written for Building America practitioners and HVAC contractors and installers. It includes a compilation of information provided by manufacturers, researchers, and the Department of Energy as well as recent research results from the Partnership for Advanced Residential Retrofit (PARR) Building America team.

  5. Waste and dust utilisation in shaft furnaces

    Directory of Open Access Journals (Sweden)

    Senk, D.

    2005-12-01

    Full Text Available Wastes and dusts from steel industry, non-ferrous metallurgy and other branches can be utilized e.g. in agglomeration processes (sintering, pelletizing or briquetting and by injection into shaft furnaces. This paper deals with the second way. Combustion and reduction behaviour of iron- and carbon-rich metallurgical dusts and sludges containing lead, zinc and alkali as well as other wastes with and without pulverized coal (PC has been studied when injecting into shaft furnaces. Following shaft furnaces have been examined: blast furnace, cupola furnace, OxiCup furnace and imperial-smelting furnace. Investigations have been done at laboratory and industrial scale. Some dusts and wastes under certain conditions can be not only reused but can also improve combustion efficiency at the tuyeres as well as furnace performance and productivity.

    Los residuos y polvos de filtro provenientes de la industria siderúrgica, de la obtención de metales no ferrosos y de otras industrias, pueden ser utilizados, por ejemplo, en procesos de aglomeración como sintetizado, peletizado o briqueteado. En su caso, estos pueden ser inyectados en los hornos de cuba. Este artículo se enfoca a la inyección de estos materiales en los hornos de cuba. El comportamiento de la combustión y reducción de los polvos ricos en hierro y carbono y también lodos que contienen plomo, zinc y compuestos alcalinos y otros residuos con o sin carbón pulverizado (CP fue examinado, cuando se inyectaron en hornos de cuba. Los siguientes hornos de cuba fueron examinados: Horno alto, cubilote, OxiCup y horno de cuba Imperial Smelting. Las investigaciones se llevaron a cabo a escala de laboratorio e industrial. Algunos residuos y polvos bajo ciertas condiciones, no sólo pueden ser reciclados, sino también mejoran la eficiencia de combustión en las toberas, la operación y productividad del horno.

  6. Hypervelocity impacts into graphite

    Science.gov (United States)

    Latunde-Dada, S.; Cheesman, C.; Day, D.; Harrison, W.; Price, S.

    2011-03-01

    Studies have been conducted into the characterisation of the behaviour of commercial graphite (brittle) when subjected to hypervelocity impacts by a range of projectiles. The experiments were conducted with a two-stage gas gun capable of launching projectiles of differing density and strength to speeds of about 6kms-1 at right angles into target plates. The damage caused is quantified by measurements of the crater depth and diameters. From the experimental data collected, scaling laws were derived which correlate the crater dimensions to the velocity and the density of the projectile. It was found that for moderate projectile densities the crater dimensions obey the '2/3 power law' which applies to ductile materials.

  7. Effect of temperature on coke properties and CO2 reactivity under laboratory conditions and in an experimental blast furnace

    OpenAIRE

    Hilding, Tobias; Kazuberns, Kelli; Gupta, Sushil; Sahajwalla, Veena; Sakurovs, Richard; Björkman, Bo; Wikström, Jan-Olov

    2005-01-01

    Physical and chemical properties of coke samples excavated from LKAB's Experimental Blast Furnace (EBF) at MEFOS in Lulea, Sweden were characterized. A thermal annealing study the raw coke used in the EBF was also conducted in a horizontal furnace in a neutral environment at a range of temperatures up to 1650DGC. Carbon crystallite height of the EBF coke and of the cokes treated in the laboratory furnace were measured by XRD while mineral phases were characterized by using SEM/EDS. The CO2 re...

  8. Sampling

    CERN Document Server

    Thompson, Steven K

    2012-01-01

    Praise for the Second Edition "This book has never had a competitor. It is the only book that takes a broad approach to sampling . . . any good personal statistics library should include a copy of this book." —Technometrics "Well-written . . . an excellent book on an important subject. Highly recommended." —Choice "An ideal reference for scientific researchers and other professionals who use sampling." —Zentralblatt Math Features new developments in the field combined with all aspects of obtaining, interpreting, and using sample data Sampling provides an up-to-date treat

  9. Optical properties of graphite oxide and reduced graphite oxide

    Science.gov (United States)

    Jung, Eilho; Lee, Seokbae; Roh, Seulki; Hwang, Eunhee; Lee, Junghyun; Lee, Hyoyoung; Hwang, Jungseek

    2014-07-01

    We studied the optical properties of a graphite oxide and a reduced graphite oxide by using the optical spectroscopic technique. The graphite oxide does not show a finite dc conductivity and has several characteristic absorption modes in the mid-infrared region, caused by an epoxide functional group and hydroxyl and carboxyl moieties in the mid-infrared range. The reduced graphite oxide shows a Drude-like response in the far-infrared region and the estimated dc conductivity and electric mobility are around 200 Ω-1cm-1 and ˜100 cm2V-1s-1, respectively. We found that the optical conductivity cannot be fitted with a simple Drude model, which indicates that the charge carriers are correlated. We applied an extended Drude model and obtained the optical scattering rate and the optical effective mass. We found that the optical effective mass can carry information of both the enhanced mass by correlation and the electronic band structure.

  10. High-Temperature (940 °C) furnace in 18/20 T cold bore magnet

    Science.gov (United States)

    Wang, Ze; Hou, Yubin; Feng, Qiyuan; Dong, Hongliang; Lu, Qingyou

    2018-01-01

    We present a high-temperature furnace that can work continuously in an 18/20 T cold bore magnet. A specially designed liquid nitrogen (LN2) jacket is between the high-temperature parts of the furnace and the liquid helium in the magnet Dewar. With LN2 serving as the cooling medium, the calculated value of radiation received by the liquid helium (LHe) is as low as 0.004 W. The furnace can be put into LHe Dewar directly. Together with the magnet, the furnace can provide experimental conditions of a strong static magnetic field and temperatures up to 940 °C. A cobalt oxide synthesis in solution was carried out at 200 °C with and without a 15 T magnetic field for 8 h. Differences in material structure with the applied field were observed in transmission electron micrographs of the products. A Co film sample was treated at 900 °C with and without a 6.8 T magnetic field for 30 min. The scanning electron micrographs of the treated samples show that magnetic field had a clear effect on the heat treatment process. These two applications confirmed the performance of the furnace both in high magnetic field and at high temperature.

  11. ROTARY FURNACES FOR THERMAL PROCESSING AND DRYING OF POLYDISPERSE MATERIALS

    Directory of Open Access Journals (Sweden)

    S. L. Rovin

    2006-01-01

    Full Text Available It is shown that rotary furnaces and drying ovens are a perspective type of furnaces, allowing to solve a number of problems in conditions of flexible production and strong resources economy

  12. Characterization study of electric arc furnace dust phases

    Directory of Open Access Journals (Sweden)

    Janaína Gonçalves Maria da Silva Machado

    2006-03-01

    Full Text Available Electric arc furnace dust (EAFD is a solid waste generated in the collection of particulate material during steelmaking process in electric arc furnace. The aim of this work is to carry out a chemical and structural characterization of two EAFD samples with different Zn contents. Optical emission spectroscopy via inductively coupled plasma (ICP, X ray diffractometry (XRD and Mössbauer spectroscopy analysis were carried out in such EAFD samples. From XRD measurements, the samples exhibits the following phases: ZnFe2O4, Fe3O4, MgFe2O4, FeCr2O4, Ca0.15Fe2.85O4, MgO, Mn3O4, SiO2 and ZnO. The phases detected by Mössbauer spectroscopy were: ZnFe2O4, Fe3O4, Ca0.15Fe2.85O4 and FeCr2O4. Magnesium ferrite (MgFe2O4, observed in the XRD patterns as overlapped peaks, was not identified in the Mössbauer spectroscopy analysis.

  13. INVESTIGATIONS ON OPERATION OF ROTARY TILTING FURNACES

    Directory of Open Access Journals (Sweden)

    S. L. Rovin

    2016-01-01

    Full Text Available Rotary tilting furnace (RTF is a new type of fuel furnaces, that provide the most efficient heating and recycling of polydisperse materials. The paper describes results of the investigations on thermal processes in the RTF, movement of materials and non-isothermal gas flow during kiln rotary process. The investigations have been carried out while using physical and computer simulations and under actual operating conditions applying the pilot plant. Results of the research have served as a basis for development of recommendations on the RTF calculations and designing and they have been also used for constructional design of a rotary tilting furnace for heating and melting of cast iron chips, reduction smelting of steel mill scale, melting of aluminum scrap, melting of lead from battery scrap. These furnaces have a high thermal efficiency (~50 %, technological flexibility, high productivity and profitability. Proven technical solutions for recycling of ferrous and non-ferrous metals develop the use of RTF in the foundry and metallurgical industry as the main technological unit for creation of cost-effective small-tonnage recycling of metal waste generated at the plants. The research results open prospects for organization of its own production for high-quality charging material in Belarus in lieu of imported primary metal. The proposed technology makes it possible to solve environmental challenge pertaining to liquidation of multi-tonnage heaps of metal-containing wastes.

  14. Energy Saving Devices on Gas Furnaces.

    Science.gov (United States)

    1980-03-01

    DEVICES FOR GAS FURNACES THOMAS E. BRISBANE ,o"’ P. B. SHEPHERD JOHNS-MANVILLE SALES CORPORATION RESEARCH & DEVELOPMENT CENTER KEN- CARYL RANCH, DENVER...by Mr. Thomas E. Brisbane under the direction of Dr. S. Karaki, Professor of Civil Engineering and Director, Solar Energy Application Laboratory. Mr

  15. Protecting brazing furnaces from air leaks

    Science.gov (United States)

    Armenoff, C. T.; Mckown, R. D.

    1980-01-01

    Inexpensive inert-atmosphere shielding protects vacuum brazing-furnace components that are likely to spring leak. Pipefittings, gages, and valves are encased in transparent plastic shroud inflated with argon. If leak develops, harmless argon will enter vacuum chamber, making it possible to finish ongoing brazing or heat treatment before shutting down for repair.

  16. Calibration procedure for fire resistance furnaces

    NARCIS (Netherlands)

    Twilt, L.; Leur, P.H.E. van de; Wickström, U.

    1996-01-01

    On behalf of CEN/TC 127 "Fire Safety in Buildings", a series of tests has been carried out to evaluate and complete the draft calibration procedure for fire resistance furnaces [4]. Fourteen laboratories in nine European countries participated in the test series, each carrying out one calibration

  17. REACTIVATION OF FERRIC OXIDES IN ROTARY FURNACES

    Directory of Open Access Journals (Sweden)

    S. L. Rovin

    2011-01-01

    Full Text Available The advantages of rotary furnaces, developed by specialists of GGTU named after P. O. Suhoj and UP «Tehnolit» for carrying out of ferric oxide recycling with regard to conditions of the Republic of Belarus, are described.

  18. Graphite oral tattoo: case report

    National Research Council Canada - National Science Library

    Moraes, Renata Mendonça; Gouvêa Lima, Gabriela de Morais; Guilhermino, Marinaldo; Vieira, Mayana Soares; Carvalho, Yasmin Rodarte; Anbinder, Ana Lia

    2015-01-01

    .... We report a rare case of a graphite tattoo on the palate of a 62-year-old patient with a history of pencil injury, compare it with amalgam tattoos, and determine the prevalence of oral tattoos...

  19. Design and Testing of a Cupola Furnace for Micheal Okpara ...

    African Journals Online (AJOL)

    ... for the present study. It is thus recommended that this novelty design be used as a foundation for building bigger furnaces and for the sensitisation of students' awareness in foundry technology and practices. Keywords: furnace lining, refractory materials, critical radius of insulation, furnace fuel, heat transfer, cupola zones ...

  20. Thermal Analysis of an Industrial Furnace

    Directory of Open Access Journals (Sweden)

    Mirko Filipponi

    2016-10-01

    Full Text Available Industries, which are mainly responsible for high energy consumption, need to invest in research projects in order to develop new managing systems for rational energy use, and to tackle the devastating effects of climate change caused by human behavior. The study described in this paper concerns the forging industry, where the production processes generally start with the heating of steel in furnaces, and continue with other processes, such as heat treatments and different forms of machining. One of the most critical operations, in terms of energy loss, is the opening of the furnace doors for insertion and extraction operations. During this time, the temperature of the furnaces decreases by hundreds of degrees in a few minutes. Because the dispersed heat needs to be supplied again through the combustion of fuel, increasing the consumption of energy and the pollutant emissions, the evaluation of the amount of lost energy is crucial for the development of systems which can contain this loss. To perform this study, CFD simulation software was used. Results show that when the door opens, because of temperature and pressure differences between the furnace and the ambient air, turbulence is created. Results also show that the amount of energy lost for an opening of 10 min for radiation, convection and conduction is equal to 5606 MJ where convection is the main contributor, with 5020 MJ. The model created, after being validated, has been applied to perform other simulations, in order to improve the energy performance of the furnace. Results show that reducing the opening time of the door saves energy and limits pollutant emissions.

  1. Technical Update: Johnson Space Center system using a solid electrolytic cell in a remote location to measure oxygen fugacities in CO/CO2 controlled-atmosphere furnaces

    Science.gov (United States)

    Jurewicz, A. J. G.; Williams, R. J.; Le, L.; Wagstaff, J.; Lofgren, G.; Lanier, A.; Carter, W.; Roshko, A.

    1993-01-01

    Details are given for the design and application of a (one atmosphere) redox-control system. This system differs from that given in NASA Technical Memorandum 58234 in that it uses a single solid-electrolytic cell in a remote location to measure the oxygen fugacities of multiple CO/CO2 controlled-atmosphere furnaces. This remote measurement extends the range of sample-furnace conditions that can be measured using a solid-electrolytic cell, and cuts costs by extending the life of the sensors and by minimizing the number of sensors in use. The system consists of a reference furnace and an exhaust-gas manifold. The reference furnace is designed according to the redox control system of NASA Technical Memorandum 58234, and any number of CO/CO2 controlled-atmosphere furnaces can be attached to the exhaust-gas manifold. Using the manifold, the exhaust gas from individual CO/CO2 controlled atmosphere furnaces can be diverted through the reference furnace, where a solid-electrolyte cell is used to read the ambient oxygen fugacity. The oxygen fugacity measured in the reference furnace can then be used to calculate the oxygen fugacity in the individual CO/CO2 controlled-atmosphere furnace. A BASIC computer program was developed to expedite this calculation.

  2. High temperature coke characteristics in the blast furnace:evaluation of coke properties in the raceway area

    OpenAIRE

    Lundgren, Maria; Sundqvist Ökvist, Lena; Hyllander, Gunilla; Jansson, Björn; Björkman, Bo

    2012-01-01

    Core-drilling into the coke bed of raceway and hearth has been performed in the LKAB Experimental Blast Furnace (EBF®) during short stoppages aiming to characterize raceway conditions corresponding to different operational conditions. All coke operation, injection of pulverized coal and injection of a mixture of coal and blast furnace flue dust (BFD) were evaluated and compared. The samples have been studied regarding particle size and distribution, coke have been evaluated with chemical comp...

  3. AUTOMATION OF GLASS TEMPERING FURNACE BY USING PLC

    Directory of Open Access Journals (Sweden)

    Abdullah BÜYÜKYILDIZ

    2007-02-01

    Full Text Available In this study, a furnace which is used for observation of environments under high temperature, and also used for manufacturing of glasses which are resisted to high temperature has been designed and implemented. Automation of this system has been done by using PLC. Operating parameters of furnace such as materials entering, the furnace, the local temperature control of furnace, cooling control and materials outing have been sensed with Hall Effect Sensor. Furthermore, the observation of parameters of furnace on screen has been provided with SCADA software. Obtained products have been shown the system works successfully.

  4. Assessment of homogeneity and minimum sample mass for cadmium analysis in powdered certified reference materials and real rice samples by solid sampling electrothermal vaporization atomic fluorescence spectrometry.

    Science.gov (United States)

    Mao, Xuefei; Liu, Jixin; Huang, Yatao; Feng, Li; Zhang, Lihua; Tang, Xiaoyan; Zhou, Jian; Qian, Yongzhong; Wang, Min

    2013-01-30

    To optimize analytical quality controls of solid sampling electrothermal vaporization atomic fluorescence spectrometry (SS-ETV-AFS), the homogeneity (H(E)) of rice samples and their minimum sample mass (M) for cadmium analysis were evaluated using three certified reference materials (CRMs) and real rice samples. The effects of different grinding degrees (particle sizes 1 mm) on H(E) and M of real rice samples were also investigated. The calculated M values of three CRMs by the Pauwels equation were 2.19, 19.76, and 3.79 mg. The well-ground real rice samples (particle size method were compared with the results by microwave digestion graphite furnace atomic absorption spectrometry with a 0.5 g sample mass. There was no significant difference between these two methods, which meant that SS-ETV-AFS could be used to accurately detect Cd in rice with several milligrams of samples instead of the certified value (200 mg) or the recommended mass (200-500 mg) of the methods of the Association of Official Analytical Chemists.

  5. Effect of temperature on the graphitization process of a semianthracite

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez, D.; Montes-Moran, M.A.; Garcia, A.B. [Instituto Nacional del Carbon, CSIC, Apdo. 73, 33080 Oviedo (Spain); Young, R.J. [Manchester Materials Science Centre, UMIST/University of Manchester, Grosvenor St., M1 7HS Manchester (United Kingdom)

    2002-12-01

    In this work, a Spanish semianthracite was graphitized at temperatures {>=}2400 C. The aim of this research was to study the influence of the temperature on the evolution of the structural order of the graphitic materials obtained. Crystalline parameters such as interlayer spacing, d{sub 002}, and domain sizes L{sub c} and L{sub a} were calculated from X-ray diffraction (XRD) measurements. The intensity ratio of the D and G Raman bands was used to assess the degree of orientation of these materials. Analysis of the XRD and Raman data of the graphitized samples allowed one to conclude that their structural order tend to increase with the temperature of treatment. Interlayer distances d{sub 002} remained almost unchanged in the whole range of temperatures studied. It seems that after a given value of this parameter is reached, improvement of samples' crystallinity is only related to crystallite-size growth. According to the Raman I{sub D}/I{sub D}+I{sub G} ratio, an increase of the bidimensional structural order with the graphitization temperature is observed. The degree of graphitization achieved at the highest temperature employed can be improved by increasing the time of treatment.

  6. Effective Thermal Conductivity of Graphite Materials with Cracks

    Science.gov (United States)

    Pestchaanyi, S. E.; Landman, I. S.

    The dependence of effective thermal diffusivity on temperature caused by volumetric cracks is modelled for macroscopic graphite samples using the three-dimensional thermomechanics code Pegasus-3D. At high off-normal heat loads typical of the divertor armour, thermostress due to the anisotropy of graphite grains is much larger than that due to the temperature gradient. Numerical simulation demonstrated that the volumetric crack density both in fine grain graphites and in the CFC matrix depends mainly on the local sample temperature, not on the temperature gradient. This allows to define an effective thermal diffusivity for graphite with cracks. The results obtained are used to explain intense cracking and particle release from carbon based materials under electron beam heat load. Decrease of graphite thermal diffusivity with increase of the crack density explains particle release mechanism in the experiments with CFC where a clear energy threshold for the onset of particle release has been observed in J. Linke et al. Fusion Eng. Design, in press, Bazyler et al., these proceedings. Surface temperature measurement is necessary to calibrate the Pegasus-3D code for simulation of ITER divertor armour brittle destruction.

  7. Fabrication of graphene from graphite by a thermal assisted vacuum arc discharge system

    Science.gov (United States)

    Cheng, Guo-Wei; Chu, Kevin; Chen, Jeng Shiung; Tsai, Jeff T. H.

    2017-04-01

    In this study, graphene was fabricated on copper foils using a high temperature furnace embedded in a vacuum arc discharge method. Combining the advantages of chemical vapor deposition and vacuum arc discharge, single-layer graphene can be fabricated at 600 °C base temperature from the mini furnace embedded with a fast heating via the photon radiation from the vacuum arc to 1100 °C on the substrates' surface. The optimal fabrication condition was determined through a series of experiments on ambient pressure, processing time, arc currents, and the cooling process. Observations by scanning electron microscopy, Raman spectroscopy, and optical microscopy showed that the main products were single-layer graphene, which has a uniform thickness across the entire substrate. The results demonstrated that the combination of a vacuum arc with a thermal method that uses graphite as a carbon source provides a low-cost and straight forward method to synthesize graphene films for graphene-based applications.

  8. The effect of heating power on impurity formation and transport during the holding phase in a Bridgman furnace for directional solidification of multi-crystalline silicon

    Science.gov (United States)

    Ellingsen, Kjerstin; Lindholm, Dag; M`Hamdi, Mohammed

    2016-06-01

    Oxygen and carbon are the most common impurities in multi-crystalline silicon. The general mechanism for formation and transport of O and C in the solidification furnace is as follows: oxygen from the silica crucible comes into the melt and combines with a silicon atom and evaporates at the gas/melt interface in the form of silicon oxide (SiO). Argon inert gas, injected into the furnace chamber, carries the SiO to the hot graphite fixtures, where it reacts with carbon to form carbon monoxide (CO) and silicon carbide (SiC). CO is carried by the gas to the melt free surface, where it dissociates into carbon and oxygen. Finally, during solidification oxygen and carbon are incorporated into the crystal. A global furnace model accounting for heat transfer, melt flow, gas flow and impurity transport has been applied to investigate the oxygen and carbon formation and transport in a vertical Bridgman furnace during the holding phase when the furnace is at its hottest. A case study is performed to investigate the effect of the applied heating power on the carbon and oxygen concentrations in the melt prior to solidification.

  9. Mineralogical and isotopic characterization of graphite deposits from the Anatectic Complex of Toledo, central Spain

    Science.gov (United States)

    Martín-Méndez, Iván; Boixereu, Ester; Villaseca, Carlos

    2016-06-01

    Graphite is found dispersed in high-grade metapelitic rocks of the Anatectic Complex of Toledo (ACT) and was mined during the mid twentieth century in places where it has been concentrated (Guadamur and la Puebla de Montalbán mines). Some samples from these mines show variable but significant alteration intensity, reaching very low-T hydrothermal (supergene) conditions for some samples from the waste heap of the Guadamur site (<100 °C and 1 kbar). Micro-Raman and XRD data indicate that all the studied ACT graphite is of high crystallinity irrespective of the degree of hydrothermal alteration. Chemical differences were obtained for graphite δ13C composition. ACT granulitic graphite shows δ13CPDB values in the range of -20.5 to -27.8 ‰, indicating a biogenic origin. Interaction of graphite with hydrothermal fluids does not modify isotopic compositions even in the most transformed samples from mining sites. The different isotopic signatures of graphite from the mining sites reflect its contrasted primary carbon source. The high crystallinity of studied graphite makes this area of central Spain suitable for graphitic exploration and its potential exploitation, due to the low carbon content required for its viability and its strategic applications in advanced technologies, such as graphene synthesis.

  10. Matrix effects in the determination of molybdenum in plants by carbon furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Studnicki, M.

    1979-07-01

    Molybdenum is a microelement taken by plants in lower quantities than other microelements. The effects of different acids, cations, and anions important in plant materials are analyzed. A double-beam Instrumentation Laboratory atomic absorption spectrometer Model 251 with hydrogen background corrector, a graphite furnace IL 455, and Dohrmann Envirotech recorder Model SC 1200 were used. Acids strongly influence the Mo signal. Most of the phosphoric acid in the range 0.01 to 1% increased the signal. Ammonium salts of these acids also changed the Mo signal, but the sign of the change may be other than for the acids (for example, ammonium nitrates). Calcium chloride strongly decreased the signal. This influence was reduced in the presence of ammonium phosphate and the disodium salt of EDTA. 5 figures.

  11. GAS MOVEMENT IN ROTARY TILTING FURNACES

    Directory of Open Access Journals (Sweden)

    S. L. Rovin

    2016-01-01

    Full Text Available The article presents the results of studies of gas movement and heat and mass transfer processes in the rotary tilting furnace (RTF at the heat treatment of disperse materials. The study was performed through computer modeling using software packages ANSYS CFX and Solid Works Flow Simulation. The results were used to design RTF with different capacity and application and helped to improve their technical and economic characteristics.

  12. Chemically reduced graphene contains inherent metallic impurities present in parent natural and synthetic graphite

    Science.gov (United States)

    Ambrosi, Adriano; Chua, Chun Kiang; Khezri, Bahareh; Sofer, Zdeněk; Webster, Richard D.; Pumera, Martin

    2012-01-01

    Graphene-related materials are in the forefront of nanomaterial research. One of the most common ways to prepare graphenes is to oxidize graphite (natural or synthetic) to graphite oxide and exfoliate it to graphene oxide with consequent chemical reduction to chemically reduced graphene. Here, we show that both natural and synthetic graphite contain a large amount of metallic impurities that persist in the samples of graphite oxide after the oxidative treatment, and chemically reduced graphene after the chemical reduction. We demonstrate that, despite a substantial elimination during the oxidative treatment of graphite samples, a significant amount of impurities associated to the chemically reduced graphene materials still remain and alter their electrochemical properties dramatically. We propose a method for the purification of graphenes based on thermal treatment at 1,000 °C in chlorine atmosphere to reduce the effect of such impurities on the electrochemical properties. Our findings have important implications on the whole field of graphene research. PMID:22826262

  13. Thermal Pyrolytic Graphite Enhanced Components

    Science.gov (United States)

    Hardesty, Robert E. (Inventor)

    2015-01-01

    A thermally conductive composite material, a thermal transfer device made of the material, and a method for making the material are disclosed. Apertures or depressions are formed in aluminum or aluminum alloy. Plugs are formed of thermal pyrolytic graphite. An amount of silicon sufficient for liquid interface diffusion bonding is applied, for example by vapor deposition or use of aluminum silicon alloy foil. The plugs are inserted in the apertures or depressions. Bonding energy is applied, for example by applying pressure and heat using a hot isostatic press. The thermal pyrolytic graphite, aluminum or aluminum alloy and silicon form a eutectic alloy. As a result, the plugs are bonded into the apertures or depressions. The composite material can be machined to produce finished devices such as the thermal transfer device. Thermally conductive planes of the thermal pyrolytic graphite plugs may be aligned in parallel to present a thermal conduction path.

  14. Method of Joining Graphite Fibers to a Substrate

    Science.gov (United States)

    Beringer, Durwood M. (Inventor); Caron, Mark E. (Inventor); Taddey, Edmund P. (Inventor); Gleason, Brian P. (Inventor)

    2014-01-01

    A method of assembling a metallic-graphite structure includes forming a wetted graphite subassembly by arranging one or more layers of graphite fiber material including a plurality of graphite fibers and applying a layer of metallization material to ends of the plurality of graphite fibers. At least one metallic substrate is secured to the wetted graphite subassembly via the layer of metallization material.

  15. Reduce Air Infiltration in Furnaces (English/Chinese) (Fact Sheet)

    Energy Technology Data Exchange (ETDEWEB)

    2011-10-01

    Chinese translation of the Reduce Air Infiltration in Furnaces fact sheet. Provides suggestions on how to improve furnace energy efficiency. Fuel-fired furnaces discharge combustion products through a stack or a chimney. Hot furnace gases are less dense and more buoyant than ambient air, so they rise, creating a differential pressure between the top and the bottom of the furnace. This differential, known as thermal head, is the source of a natural draft or negative pressure in furnaces and boilers. A well-designed furnace (or boiler) is built to avoid air leakage into the furnace or leakage of flue gases from the furnace to the ambient. However, with time, most furnaces develop cracks or openings around doors, joints, and hearth seals. These openings (leaks) usually appear small compared with the overall dimensions of the furnace, so they are often ignored. The negative pressure created by the natural draft (or use of an induced-draft fan) in a furnace draws cold air through the openings (leaks) and into the furnace. The cold air becomes heated to the furnace exhaust gas temperature and then exits through the flue system, wasting valuable fuel. It might also cause excessive oxidation of metals or other materials in the furnaces. The heat loss due to cold air leakage resulting from the natural draft can be estimated if you know four major parameters: (1) The furnace or flue gas temperature; (2) The vertical distance H between the opening (leak) and the point where the exhaust gases leave the furnace and its flue system (if the leak is along a vertical surface, H will be an average value); (3) The area of the leak, in square inches; and (4) The amount of operating time the furnace spends at negative pressure. Secondary parameters that affect the amount of air leakage include these: (1) The furnace firing rate; (2) The flue gas velocity through the stack or the stack cross-section area; (3) The burner operating conditions (e.g., excess air, combustion air temperature

  16. Characterization of an hrp-aox-polyaniline-graphite composite biosensor

    Directory of Open Access Journals (Sweden)

    Ana Carolina O. Santana

    2014-12-01

    Full Text Available Nowadays there is an increasing demand to develop new and robust biosensors in order to detect low concentrations of different chemicals, in practical and small devices, giving fast and confident responses. The electrode material was a polyaniline-graphite-epoxy composite (PANI/GEC. Alcohol oxidase (AOX and horseradish peroxidase (HRP enzymes were immobilized and the responses were tested by cyclic voltammetry. The conductivities for the composites of graphite/polyaniline were determined. The cyclic voltammograms allowed detecting ethanol in pure diluted samples in a range from 0.036 to 2.62 M. Differential scanning calorimetry (DSC and thermal gravimetry analysis (TGA were used to verify the thermal characteristics of the composites (0, 10, 20, 30 and 100 % of graphite. The Imax value was determined for the dual enzyme biosensor (0.0724 mA, and the Kapp m  as 1.41 M (with R2 =0.9912.

  17. GRAFEC: A New Spanish Program to Investigate Waste Management Options for Radioactive Graphite - 12399

    Energy Technology Data Exchange (ETDEWEB)

    Marquez, Eva; Pina, Gabriel; Rodriguez, Marina [CIEMAT, Av. Complutense, 22, 28040-MADRID (Spain); Fachinger, Johannes; Grosse, Karl-Heinz [Furnaces Nuclear Application Grenoble SAS (FNAG), 4, avenue Charles de Gaulle, 38800 Le Pont de Claix (France); Leganes Nieto, Jose Luis; Quiros Gracian, Maria [ENRESA, C/ Emilio Vargas,7 - 28043 - MADRID (Spain); Seemann, Richard [ALD Vacuum Technologies GmbH, Wilhelm-Rohn-Strasse 35, 63450 Hanau (Germany)

    2012-07-01

    encapsulation of the graphite in a long term stable glass matrix. The principal applicability has been already proved by FNAG. Crushed graphite mixed with a suitable glass powder has been pressed at elevated temperature under vacuum. The vacuum is required to avoid gas enclosures in the obtained product. The obtained products, named IGM for 'Impermeable Graphite Matrix', have densities above 99% of theoretical density. The amount of glass has been chosen with respect to the pore volume of the former graphite parts. The method allows the production of encapsulated graphite without increasing the disposal volume. This paper will give a short overview of characterisation results of different irradiated graphite materials obtained at CIEMAT and in the Carbowaste project as well as the proposed methods and the actual status of the program including first results about leaching of non-radioactive IGM samples and hopefully first tendencies concerning the C-14 separation from graphite of Vandellos I by thermal treatment. Both processes, the thermal treatment as well as the IGM, have the potential to solve problems related to the management of irradiated graphite in Spain. However the methods have only been tested with different types of i-graphite and virgin graphite, respectively. Only investigations with real i-graphite from Spain will reveal whether the described methods are applicable to graphite from Vandellos I. However all partners are convinced that one of these new methods or a combination of them will lead to a feasible option to manage i-graphite in Spain on an industrial scale. (authors)

  18. Advanced Surface and Microstructural Characterization of Natural Graphite Anodes for Lithium Ion Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Gallego, Nidia C [ORNL; Contescu, Cristian I [ORNL; Meyer III, Harry M [ORNL; Howe, Jane Y [ORNL; Meisner, Roberta Ann [ORNL; Payzant, E Andrew [ORNL; Lance, Michael J [ORNL; Yoon, Steve [A123 Systems, Inc.; Denlinger, Matthew [A123 Systems, Inc.; Wood III, David L [ORNL

    2014-01-01

    Natural graphite powders were subjected to a series of thermal treatments in order to improve the anode irreversible capacity loss (ICL) and capacity retention during long-term cycling of lithium ion batteries. A baseline thermal treatment in inert Ar or N2 atmosphere was compared to cases with a proprietary additive to the furnace gas environment. This additive substantially altered the surface chemistry of the natural graphite powders and resulted in significantly improved long-term cycling performance of the lithium ion batteries over the commercial natural graphite baseline. Different heat-treatment temperatures were investigated ranging from 950-2900 C with the intent of achieving the desired long-term cycling performance with as low of a maximum temperature and thermal budget as possible. A detailed summary of the characterization data is also presented, which includes X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and temperature-programed desorption mass spectroscopy (TPD-MS). This characterization data was correlated to the observed capacity fade improvements over the course of long-term cycling at high charge-discharge rates in full lithium-ion coin cells. It is believed that the long-term performance improvements are a result of forming a more stable solid electrolyte interface (SEI) layer on the anode graphite surfaces, which is directly related to the surface chemistry modifications imparted by the proprietary gas environment during thermal treatment.

  19. Separation medium containing thermally exfoliated graphite oxide

    Science.gov (United States)

    Prud'homme, Robert K. (Inventor); Aksay, Ilhan A. (Inventor); Herrera-Alonso, Margarita (Inventor)

    2012-01-01

    A separation medium, such as a chromatography filling or packing, containing a modified graphite oxide material, which is a thermally exfoliated graphite oxide with a surface area of from about 300 m.sup.2/g to 2600 m.sup.2/g, wherein the thermally exfoliated graphite oxide has a surface that has been at least partially functionalized.

  20. Photoemission study of K on graphite

    NARCIS (Netherlands)

    Bennich, P.; Puglia, C.; Brühwiler, P.A.; Nilsson, A.; Sandell, A.; Mårtensson, N.; Rudolf, P.

    1999-01-01

    The physical and electronic structure of the dispersed and (2×2) phases of K/graphite have been characterized by valence and core-level photoemission. Charge transfer from K to graphite is found to occur at all coverages, and includes transfer of charge to the second graphite layer. A rigid band

  1. The influence of buoyant forces and volume fraction of particles on the particle pushing/entrapment transition during directional solidification of Al/SiC and Al/graphite composites

    Science.gov (United States)

    Stefanescu, Doru M.; Moitra, Avijit; Kacar, A. Sedat; Dhindaw, Brij K.

    1990-01-01

    Directional solidification experiments in a Bridgman-type furnace were used to study particle behavior at the liquid/solid interface in aluminum metal matrix composites. Graphite or silicon-carbide particles were first dispersed in aluminum-base alloys via a mechanically stirred vortex. Then, 100-mm-diameter and 120-mm-long samples were cast in steel dies and used for directional solidification. The processing variables controlled were the direction and velocity of solidification and the temperature gradient at the interface. The material variables monitored were the interface energy, the liquid/particle density difference, the particle/liquid thermal conductivity ratio, and the volume fraction of particles. These properties were changed by selecting combinations of particles (graphite or silicon carbide) and alloys (Al-Cu, Al-Mg, Al-Ni). A model which consideres process thermodynamics, process kinetics (including the role of buoyant forces), and thermophysical properties was developed. Based on solidification direction and velocity, and on materials properties, four types of behavior were predicted. Sessile drop experiments were also used to determine some of the interface energies required in calculation with the proposed model. Experimental results compared favorably with model predictions.

  2. How to convert biological carbon into graphite for AMS

    Energy Technology Data Exchange (ETDEWEB)

    Getachew, G; Kim, S; Burri, B J; Kelly, P B; Haack, K W; Ognibene, T J; Buchholz, B A; Vogel, J S; Modrow, J; Clifford, A J

    2006-07-27

    Isotope tracer studies, particularly radiocarbon measurements, play a key role in biological, nutritional, and environmental research. Accelerator mass spectrometry (AMS) is now the most sensitive detection method for radiocarbon, but AMS is not widely used in kinetic studies of humans. Part of the reason is the expense, but costs would decrease if AMS were used more widely. One component in the cost is sample preparation for AMS. Biological and environmental samples are commonly reduced to graphite before they are analyzed by AMS. Improvements and mechanization of this multi-step procedure is slowed by a lack of organized educational materials for AMS sample preparation that would allow new investigators to work with the technique without a substantial outlay of time and effort. We present a detailed sample preparation protocol for graphitizing biological samples for AMS and include examples of nutrition studies that have used this procedure.

  3. Melting and casting of alloys in a solar furnace

    Energy Technology Data Exchange (ETDEWEB)

    Suresh, D. (Indian Inst. of Science, Bangalore, India); Rohatgi, P.K.

    1979-01-01

    A feasibility study conducted using a small working model of a solar furnace is reported in which the melting and casting of various alloys was tested. The prototype furnace had either a spun copper or aluminum hemispherical concentrator, and was manually tracked. A later self-tracking version consisted of a paraboloidal cofiguration fabricated from a wire mesh antenna covered with aluminized polyester. The experimental results show that a simple and inexpensive solar furnace could be commercialized in the near future. (SPH)

  4. Pellet reduction properties under different blast furnace operating conditions

    OpenAIRE

    Leimalm, Ulrika

    2006-01-01

    One of the aims of modern blast furnace (BF) ironmaking is to reduce coke consumption. One way is to increase the injection of reduction agents, such as pulverized coal. An increase in pulverized coal injection rate (PCR) will affect the blast furnace process and the conditions for iron oxide reduction. Changes in PCR influence the composition of the ascending gases and the in-furnace temperature isotherms. The performed tests involve full-scale, pilot and laboratory investigations. Raw mater...

  5. Graphite oral tattoo: case report.

    Science.gov (United States)

    Moraes, Renata Mendonça; Gouvêa Lima, Gabriela de Morais; Guilhermino, Marinaldo; Vieira, Mayana Soares; Carvalho, Yasmin Rodarte; Anbinder, Ana Lia

    2015-10-16

    Pigmented oral lesions compose a large number of pathological entities, including exogenous pigmentat oral tattoos, such as amalgam and graphite tattoos. We report a rare case of a graphite tattoo on the palate of a 62-year-old patient with a history of pencil injury, compare it with amalgam tattoos, and determine the prevalence of oral tattoos in our Oral Pathology Service. We also compare the clinical and histological findings of grafite and amalgam tattoos. Oral tattoos affect women more frequently in the region of the alveolar ridge. Graphite tattoos occur in younger patients when compared with the amalgam type. Histologically, amalgam lesions represent impregnation of the reticular fibers of vessels and nerves with silver, whereas in cases of graphite tattoos, this impregnation is not observed, but it is common to observe a granulomatous inflammatory response, less evident in cases of amalgam tattoos. Both types of lesions require no treatment, but in some cases a biopsy may be done to rule out melanocytic lesions.

  6. Igneous Graphite in Enstatite Chondrites

    Science.gov (United States)

    Rubin, Alan E.

    1997-01-01

    Igneous graphite. a rare constituent in terrestrial mafic and ultramafic rocks. occurs in three EH and one EL enstatite chondrite impact-melt breccias as 2-150 Ilm long euhedrallaths. some with pyramidal terminations. In contrast. graphite in most enstatite chondrites exsolved from metallic Fe-Ni as polygonal. rounded or irregular aggregates. Literature data for five EH chondrites on C combusting at high temperatures show that Abee contains the most homogeneous C isotopes (i.e. delta(sup 13)C = -8.1+/-2.1%); in addition. Abee's mean delta(sup l3)C value is the same as the average high-temperature C value for the set of five EH chondrites. This suggests that Abee scavenged C from a plurality of sources on its parent body and homogenized the C during a large-scale melting event. Whereas igneous graphite in terrestrial rocks typically forms at relatively high pressure and only moderately low oxygen fugacity (e.g., approx. 5 kbar. logfO2, approx. -10 at 1200 C ). igneous graphite in asteroidal meteorites formed at much lower pressures and oxygen fugacities.

  7. Advances in chemical and physical properties of electric arc furnace carbon steel slag by hot stage processing and mineral mixing.

    Science.gov (United States)

    Liapis, Ioannis; Papayianni, Ioanna

    2015-01-01

    Slags are recognised as a highly efficient, cost effective tool in the metal processing industry, by minimising heat losses, reducing metal oxidation through contact with air, removing metal impurities and protecting refractories and graphite electrodes. When compared to natural aggregates for use in the construction industry, slags have higher specific weight that acts as an economic deterrent. A method of altering the specific weight of EAFC slag by hot stage processing and mineral mixing, during steel production is presented in this article. The method has minimal interference with the production process of steel, even by limited additions of appropriate minerals at high temperatures. Five minerals are examined, namely perlite, ladle furnace slag, bauxite, diatomite and olivine. Measurements of specific weight are accompanied by X-ray diffraction (XRD) and fluorescence (XRF) analysis and scanning electron microscopy spectral images. It is also shown how altering the chemical composition is expected to affect the furnace refractory lining. Additionally, the process has been repeated for the most suitable mix in gas furnace and physical properties (FI, SI, LA, PSV, AAV, volume stability) examined. Alteration of the specific weight can result in tailoring slag properties for specific applications in the construction sector. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Graphite nanoreinforcements in polymer nanocomposites

    Science.gov (United States)

    Fukushima, Hiroyuki

    Nanocomposites composed of polymer matrices with clay reinforcements of less than 100 nm in size, are being considered for applications such as interior and exterior accessories for automobiles, structural components for portable electronic devices, and films for food packaging. While most nanocomposite research has focused on exfoliated clay platelets, the same nanoreinforcement concept can be applied to another layered material, graphite, to produce nanoplatelets and nanocomposites. Graphite is the stiffest material found in nature (Young's Modulus = 1060 GPa), having a modulus several times that of clay, but also with excellent electrical and thermal conductivity. The key to utilizing graphite as a platelet nanoreinforcement is in the ability to exfoliate this material. Also, if the appropriate surface treatment can be found for graphite, its exfoliation and dispersion in a polymer matrix will result in a composite with not only excellent mechanical properties but electrical properties as well, opening up many new structural applications as well as non-structural ones where electromagnetic shielding and high thermal conductivity are requirements. In this research, a new process to fabricate exfoliated nano-scale graphite platelets was established (Patent pending). The size of the resulted graphite platelets was less than 1 um in diameter and 10 nm in thickness, and the surface area of the material was around 100 m2/g. The reduction of size showed positive effect on mechanical properties of composites because of the increased edge area and more functional groups attached with it. Also various surface treatment techniques were applied to the graphite nanoplatelets to improve the surface condition. As a result, acrylamide grafting treatment was found to enhance the dispersion and adhesion of graphite flakes in epoxy matrices. The resulted composites showed better mechanical properties than those with commercially available carbon fibers, vapor grown carbon fibers

  9. Nanosecond formation of diamond and lonsdaleite by shock compression of graphite

    Science.gov (United States)

    Kraus, D.; Ravasio, A.; Gauthier, M.; Gericke, D. O.; Vorberger, J.; Frydrych, S.; Helfrich, J.; Fletcher, L. B.; Schaumann, G.; Nagler, B.; Barbrel, B.; Bachmann, B.; Gamboa, E. J.; Göde, S.; Granados, E.; Gregori, G.; Lee, H. J.; Neumayer, P.; Schumaker, W.; Döppner, T.; Falcone, R. W.; Glenzer, S. H.; Roth, M.

    2016-03-01

    The shock-induced transition from graphite to diamond has been of great scientific and technological interest since the discovery of microscopic diamonds in remnants of explosively driven graphite. Furthermore, shock synthesis of diamond and lonsdaleite, a speculative hexagonal carbon polymorph with unique hardness, is expected to happen during violent meteor impacts. Here, we show unprecedented in situ X-ray diffraction measurements of diamond formation on nanosecond timescales by shock compression of pyrolytic as well as polycrystalline graphite to pressures from 19 GPa up to 228 GPa. While we observe the transition to diamond starting at 50 GPa for both pyrolytic and polycrystalline graphite, we also record the direct formation of lonsdaleite above 170 GPa for pyrolytic samples only. Our experiment provides new insights into the processes of the shock-induced transition from graphite to diamond and uniquely resolves the dynamics that explain the main natural occurrence of the lonsdaleite crystal structure being close to meteor impact sites.

  10. Biological Kraft Chemical Recycle for Augmentation of Recovery Furnace Capacity

    Energy Technology Data Exchange (ETDEWEB)

    Stuart E. Strand

    2001-12-06

    The chemicals used in pulping of wood by the kraft process are recycled in the mill in the recovery furnace, which oxidizes organics while simultaneously reducing sulfate to sulfide. The recovery furnace is central to the economical operation of kraft pulp mills, but it also causes problems. The total pulp production of many mills is limited by the recovery furnace capacity, which cannot easily be increased. The furnace is one of the largest sources of air pollution (as reduced sulfur compounds) in the kraft pulp mill.

  11. Mechanical activation of graphite in air: A way to advanced carbon nanomaterials

    Energy Technology Data Exchange (ETDEWEB)

    Baklanova, O.N., E-mail: baklanova@ihcp.ru; Drozdov, V.A.; Lavrenov, A.V.; Vasilevich, A.V.; Muromtsev, I.V.; Trenikhin, M.V.; Arbuzov, A.B.; Likholobov, V.A.; Gorbunova, O.V.

    2015-10-15

    A high-energy planetary mill AGO-2 was used for mechanical activation of synthetic graphite with the particle size of 25–30 μm and specific surface area S{sub BET} = 3.0 m{sup 2}/g in air for 1–60 min at a 100 g acceleration of milling bodies. The X-ray diffraction, Raman spectroscopy and electron microscopy studies showed that the 60 min mechanical activation of graphite decreases the number of graphene layers in graphite crystallites to 8–12 and induces their turbostratic disorder. The size of graphite particles decreases to 6.9 μm after 30 min of mechanical activation and increases to 12.1 μm when the time of mechanical activation is extended to 60 min. Similar changes are observed for the true density of graphite: after 60 min of mechanical activation it becomes equal to 2.48 ⋅ 10{sup 3} kg/m{sup 3}, which is by 10% higher than the true density of graphite not subjected to such treatment. The specific adsorption surface of graphite (S{sub BET}) reaches its maximum values, 427–460 m{sup 2}/g, after 7–12 min of mechanical activation. A further increase in the activation time to 30–60 min decreases S{sub BET} of graphite to 230–250 m{sup 2}/g. Due to attrition of steel milling bodies caused by mechanical activation, iron is accumulated in the samples and its content exceeds 5%. Iron is distributed uniformly in the graphite as the 30–100 and 3–5 nm particles of hematite and iron carbide. The IR spectroscopy study revealed the formation of 0.8 mEq/g of the hydroxyl, phenolic, lactone and carbonyl groups on the graphite surface in the course of mechanical activation. - Highlights: • Graphite was mechanically activated in air at a 100 g acceleration of milling bodies. • The amount of graphenes in graphite crystallites decreases to 8–12. • Graphite transforms into a nanocrystalline X-ray amorphous state. • A metal–graphite composite with the 30–100 and 3–5 nm iron particles is formed. • Oxygen-containing groups in the amount of

  12. Slag wool manufacturing from blast furnace slag

    Directory of Open Access Journals (Sweden)

    Володимир Петрович Руських

    2016-11-01

    Full Text Available Slag wool is the most expensive and valuable product of blast furnace slag processing. Slag wool is in great demand nowadays. The article highlights the factors influencing the mineral wool quality: chemical composition that determines the acidity of the module, the temperature of the molten slag and the required slag jet thickness consistency. Mineral wool is produced by blowing air or steam into a jet of molten slag. As a result of it the slag crushes into droplets stretching. The resulting wool contains 5% slag and 95% air. The quality of the obtained slag wool depends on the module acidity of the slag. The blast furnace slags of «Ilyich iron and steel works of Mariupol» and «Azovstal iron & steel works» are the main (short slags – they give short fibers. To obtain high-quality long fiber wool it is necessary to add admixtures into basic blast furnace slag to reduce its basicity. As a result of the fuel and energy rising prices and the necessity to reduce the slag wool cost it is necessary to develop a new technology with fiery-liquid slag, with the removal of iron compounds and sulphur from the melts and the introduction of corrective additives to improve the quality of slag wool. Good thermal conductivity (about 0,03 kcal/m∙h∙°C and other indicators (resistance, volume weight make it possible to use the materials from slag wool (pads, rigid and semi-rigid plates as heat and sound insulating materials

  13. Carbon Tubular Morphologies in Blast Furnace Coke

    Directory of Open Access Journals (Sweden)

    Stanislav S. Gornostayev

    2008-01-01

    Full Text Available The paper reports on the first occurrence of microscale carbon tubular morphologies (CMTs in a blast furnace (BF coke. The CMTs were probably formed as a result of the conversion of solid disordered carbon via liquid phase metal particles involving a gas phase containing a substantial amount of N2 and O2. The presence of CMTs may lie behind the generation of the smallest fraction of fines in BF exhaust dust. If the amount of CMTs present in the BF exhausts gases at any particular metallurgical site proves to be substantial, it could become a subject of environmental concern.

  14. PERFORMANCE TESTING AND ANALYSIS OF CUPOLA FURNACE

    OpenAIRE

    PROF.HEMANT R. BHAGAT-PATIL; MEGHA S. LONDHEKAR

    2013-01-01

    In today’s industrial scenario huge losses/wastage occur in the manufacturing shop floor and foundry industries. The efficiency of any foundry largely depends on the efficiency of the melting process amulti-step operation where the metal is heated, treated, alloyed, and transported into die or mold cavities to form a casting. In this paper we represents the performance testing and analysis of Cupola Furnace, and reduces the problems occurs to give the best results. Our main focus in this work...

  15. Dental Porcelain Furnaces: Test and Evaluation.

    Science.gov (United States)

    1988-01-01

    Due to the low cost of this unit it should be considered for any laboratory with a moderate to high metal-ceramic fixed partial denture work load. New...either with or without vacuum. * Slow cooling cycle: This feature allows the units to be removed slowly from the muffle following the firing cycle...DEGREES HIGH TEMPERATURE 940 DEGREES TEMPERATURE RATE 55 DEG/MIN TIME AT TEMP 0.0 MINUTES REMOVAL TIME 0.3 MINUTES FURNACE TEMP 497 DEGREES CHAMBER VACUUM

  16. Slagging and Fouling Characteristics of HRSG for Ferrosilicon Electric Furnaces

    Directory of Open Access Journals (Sweden)

    Yungang Wang

    2015-02-01

    Full Text Available The slagging and fouling characteristics of the heat recovery steam generator (HRSG for ferrosilicon electric furnaces are discussed in this paper. Three ash samples were taken from the HRSG of a ferrosilicon furnace in Ningxia Province, China, which suffered from serious slagging and fouling. X-ray fluorescence (XRF, X-ray powder diffraction (XRD and scanning electron microscope (SEM were used to analyze the ash samples. The results show that low melting point salt Na2SO4 and composite salts Na (AlSi3O8 and 3K2SO4·CaSO4 deposit on the superheater tube walls in aerosol form and solidify to form the initial slag layer. With the continuous deposition of the low melting point compounds, more and more ash particles in the flue gas adhere to the slag surface to form a thicker slag. Low melting point composite salt NaO·Al2O3·SiO2 is absorbed on the evaporator tube walls in aerosol form. With the deposition of NaO·Al2O3·SiO2, more and more ash particles are absorbed to form the fouling. Since there is less space between pin-finned tubes, the large iron-rich slag particles are easily deposited on tube walls and fin surfaces, which is advantageous to the fouling process. There are large quantities of superfine ash particles in the flue gas that easily adhere to other particles or tube walls, which facilitates the slagging and fouling process.

  17. AGC-2 Graphite Preirradiation Data Package

    Energy Technology Data Exchange (ETDEWEB)

    David Swank; Joseph Lord; David Rohrbaugh; William Windes

    2012-10-01

    The NGNP Graphite R&D program is currently establishing the safe operating envelope of graphite core components for a Very High Temperature Reactor (VHTR) design. The program is generating quantitative data necessary for predicting the behavior and operating performance of the new nuclear graphite grades. To determine the in-service behavior of the graphite for pebble bed and prismatic designs, the Advanced Graphite Creep (AGC) experiment is underway. This experiment is examining the properties and behavior of nuclear grade graphite over a large spectrum of temperatures, neutron fluences and compressive loads. Each experiment consists of over 400 graphite specimens that are characterized prior to irradiation and following irradiation. Six experiments are planned with the first, AGC-1, currently being irradiated in the Advanced Test Reactor (ATR) and pre-irradiation characterization of the second, AGC-2, completed. This data package establishes the readiness of 512 specimens for assembly into the AGC-2 capsule.

  18. Voronoi-Tessellated Graphite Produced by Low-Temperature Catalytic Graphitization from Renewable Resources.

    Science.gov (United States)

    Zhao, Leyi; Zhao, Xiuyun; Burke, Luke T; Bennett, J Craig; Dunlap, Richard A; Obrovac, Mark N

    2017-09-11

    A highly crystalline graphite powder was prepared from the low temperature (800-1000 °C) graphitization of renewable hard carbon precursors using a magnesium catalyst. The resulting graphite particles are composed of Voronoi-tessellated regions comprising irregular sheets; each Voronoi-tessellated region having a small "seed" particle located near their centroid on the surface. This suggests nucleated outward growth of graphitic carbon, which has not been previously observed. Each seed particle consists of a spheroidal graphite shell on the inside of which hexagonal graphite platelets are perpendicularly affixed. This results in a unique high surface area graphite with a high degree of graphitization that is made with renewable feedstocks at temperatures far below that conventionally used for artificial graphites. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. On the low-field Hall coefficient of graphite

    Directory of Open Access Journals (Sweden)

    P. Esquinazi

    2014-11-01

    Full Text Available We have measured the temperature and magnetic field dependence of the Hall coefficient (RH in three, several micrometer long multigraphene samples of thickness between ∼9 to ∼30 nm in the temperature range 0.1 to 200 K and up to 0.2 T field. The temperature dependence of the longitudinal resistance of two of the samples indicates the contribution from embedded interfaces running parallel to the graphene layers. At low enough temperatures and fields RH is positive in all samples, showing a crossover to negative values at high enough fields and/or temperatures in samples with interfaces contribution. The overall results are compatible with the reported superconducting behavior of embedded interfaces in the graphite structure and indicate that the negative low magnetic field Hall coefficient is not intrinsic of the ideal graphite structure.

  20. Composition and method for brazing graphite to graphite

    Science.gov (United States)

    Taylor, A.J.; Dykes, N.L.

    1982-08-10

    A brazing material is described for joining graphite structures that can be used up to 2800/sup 0/C. The brazing material is formed of a paste-like composition of hafnium carbide and uranium oxide with a thermosetting resin. The uranium oxide is converted to uranium dicarbide during the brazing operation and then the hafnium carbide and uranium dicarbide form a liquid phase at a temperature about 2600/sup 0/C with the uranium diffusing and vaporizing from the joint area as the temperature is increased to about 2800/sup 0/C so as to provide a brazed joint consisting essentially of hafnium carbide. The resulting brazed joint is chemically and thermally compatible with the graphite structures.

  1. Anomalous behavior of the steel alloying elements in the genetic structure of the solid metal at its smelting in electric furnaces

    Directory of Open Access Journals (Sweden)

    Олександр Михайлович Скребцов

    2016-07-01

    Full Text Available Melting process in an electric arc furnace and transformations taking place in solidified metals are not thoroughly understood yet. This article is devoted to these phenomena in liquid and solid metal and therefore is relevant at the moment. The authors sampled molten metal during all periods of mild steel smelting in an electric arc furnace beginning from melting the charge up to metal outlet out of the furnace into the ladle. Samples were analyzed for chemical elements content, and the microstructure of solidified samples (the ratio of ferrite and pearlite. It has been found that elements expanding γ – phase domain of existence (Mn, Ni during oxidation act similarly at deoxidation, but much weaker. This fact is interesting for science, it is advisable that these phenomena should be checked for the metal melted in other melting units – induction and crucible furnaces

  2. Arsenic immobilization of Teniente furnace dust

    Energy Technology Data Exchange (ETDEWEB)

    Ichimura, R. [Japan Oil, Gas, and Metals National Corp., Kawasaki (Japan); Tateiwa, H. [Mitsui Mining and Smelting Co. Ltd., Saitama (Japan); Almendares, C. [Centro de Investigacion Minera y Metalurgica, Santiago (Chile); Sanchez, G. [CODELCO, Santiago (Chile). Division Ventanas

    2007-07-01

    A 5-year joint Japanese-Chilean project to modify the treatment of furnace dust from a converter in Chile producing harmful amounts of arsenic and lead was described. A pilot plant was constructed to evaluate the method's commercialization potential. Flue dust was recovered by a dust collector installed to capture suspended dust generated by the smelting furnace. Arsenic content was approximately 15 per cent. Ninety per cent of the arsenic was then liquidated to lixivia and dissolved by leaching flue dust with sulphuric acid. The leaching rate decreased when flue dust had a high content of residual sulfide ore. A flotation device was then incorporated in the treatment process in order to increase the copper recovery rate. A solvent recovery process was then adopted to recover the copper and zinc contained in the solution after the arsenic recovery. An economic evaluation of the process indicated that efforts should be made to improve the efficiency of the dust treatment method. 5 refs., 6 tabs., 10 figs.

  3. Quantum oscillations of the magnetic moment of graphene and graphite

    Science.gov (United States)

    Petkovic, Ivana; Lollo, Anthony; Wang, Ke; Kim, Philip; Harris, Jack

    Quantum oscillations of the magnetic moment, so called de Haas - van Alphen (dHvA) oscillations, are a powerful tool for the investigation of the Fermi surface. In graphene with a fixed carrier density, the magnetic moment is predicted to oscillate as function of increasing perpendicular field B every time the uppermost Landau level empties out, yielding the characteristic 1/B dependence. To date, it has been challenging to measure the equilibrium magnetic moment of isolated samples of graphene. In graphite a more complex oscillation sequence is observed, due to its complicated Fermi surface with both electron and hole carriers. Historically graphite was one of the first materials in which dHvA oscillations were studied, but recently interest was revived due to an observation of carriers with relativistic dynamics. We have used cantilever torque magnetometry to study diamagnetism and dHvA oscillations of isolated samples of graphene and graphite between 400 mK and 20 K. For graphite, we observe dHvA oscillations which are used to study the composition and nature of carriers. For graphene, we discuss the results in relation to relativistic dispersion and disorder.

  4. Graphite Microstructural Characterization Using Time-Domain and Correlation-Based Ultrasonics

    Energy Technology Data Exchange (ETDEWEB)

    Spicer, James [Johns Hopkins Univ., Baltimore, MD (United States)

    2017-12-06

    Among techniques that have been used to determine elastic modulus in nuclear graphites, ultrasonic methods have enjoyed wide use and standards using contacting piezoelectric tranducers have been developed to ensure repeatability of these types of measurements. However, the use of couplants and the pressures used to effectively couple transducers to samples can bias measurements and produce results that are not wholly related to the properties of the graphite itself. In this work, we have investigated the use of laser ultrasonic methods for making elastic modulus measurements in nuclear graphites. These methods use laser-based transmitters and receivers to gather data and do not require use of ultrasonic couplants or mechanical contact with the sample. As a result, information directly related to the elastic responses of graphite can be gathered even if the graphite is porous, brittle and compliant. In particular, we have demonstrated the use of laser ultrasonics for the determination of both Young’s modulus and shear modulus in a range of nuclear graphites including those that are being considered for use in future nuclear reactors. These results have been analyzed to assess the contributions of porosity and microcracking to the elastic responses of these graphites. Laser-based methods have also been used to assess the moduli of NBG-18 and IG-110 where samples of each grade were oxidized to produce specific changes in porosity. These data were used to develop new models for the elastic responses of nuclear graphites and these models have been used to infer specific changes in graphite microstructure that occur during oxidation that affect elastic modulus. Specifically, we show how ultrasonic measurements in oxidized graphites are consistent with nano/microscale oxidation processes where basal plane edges react more readily than basal plane surfaces. We have also shown the use of laser-based methods to perform shear-wave birefringence measurements and have shown

  5. Oxidation and sublimation of porous graphite during fiber laser irradiation

    Science.gov (United States)

    Phillips, Grady T.; Bauer, William A.; Gonzales, Ashley E.; Herr, Nicholas C.; Perram, Glen P.

    2017-02-01

    Porous graphite plates, cylinders and cones with densities of 1.55-1.82 g/cm3 were irradiated by a 10 kW fiber laser at 0.075 -3.525 kW/cm2 for 120 s to study mass removal and crater formation. Surface temperatures reached steady state values as high as 3767 K. The total decrease in sample mass ranged from 0.06 to 6.29 g, with crater volumes of 0.52 - 838 mm3, and penetration times for 12.7 mm thick plates as short as 38 s. Minor contaminants in the graphite samples produced calcium and iron oxide to be re-deposited on the graphite surface. Significantly increased porosity of the sample is observed even outside of the laser-irradiated region. Total mass removed increases with deposited laser energy at a rate of 4.83 g/MJ for medium extruded graphite with an apparent threshold of 0.15 MJ. Visible emission spectroscopy reveals C2 Swan and CN red, CN violet bands and Li, Na, and K 2P3/2,1/2 - 2S1/2 doublets. The reacting boundary layer is observed using a mid-wave imaging Fourier transform spectrometer (IFTS) at 2 cm-1 spectral resolution, 0.5 mm/pixel spatial resolution, and 0.75 Hz data cube rate. A two-layer radiative transfer model was used to determine plume temperature, CO, and CO2 concentrations from spectral signatures. The new understanding of graphite combustion and sublimation during laser irradiation is vital to the more complex behavior of carbon composites.

  6. Gas Desorption Behavior of Graphite Anodes in Lithium Ion Secondary Batteries After Adsorption of Electrolytes

    Science.gov (United States)

    Watanabe, Toshinori; Nobuta, Yuji; Yamauchi, Yuji; Hino, Tomoaki; Kubota, Yoshihiro; Ohzeki, Katsutomo

    When it was soaked, more were desorbed In this study, gas desorption behaviors of graphite anode samples after various surface treatments and electrolyte solvent adsorption properties were investigated. The total amount of desorbed gases for the natural graphite samples increased after soaking in propylene carbonate, and increased even further with Raman R value, suggesting that surface defects act as an effective adsorption site for the electrolyte. These findings indicate that surface treatment such as a coating might be an effective remedy to reduce the amount of desorption gases in natural graphite samples. It was also found that the total amount of gas desorption largely decreased with the coating with polymer resin and subsequent heat treatment at 423 K for 12 hours in a medium of air. It is likely that the dominant gas species present in the natural graphite after the electrolyte soaking are dependent on the binding energy and the molecular structure of the electrolyte solvent.

  7. Evaluation of co-cokes from bituminous coal with vacuum resid or decant oil, and evaluation of anthracites, as precursors to graphite

    Science.gov (United States)

    Nyathi, Mhlwazi S.

    2011-12-01

    graphitization and crystallite dimensions, of the final product is dependent on the nature of the precursor co-coke. The methodology for studying anthracites was to select two anthracites on basis of rank, PSOC1515 being semi-anthracite and DECS21 anthracite. The selected anthracites were graphitized, in both native and demineralized states, under the same conditions as co-cokes. Products obtained from DECS21 showed higher degrees of graphitization and larger crystallite dimensions than products obtained from PSOC1515. Demineralization of anthracites served to increase the degree of graphitization, indicating that the minerals contained in these anthracites have no graphitization-enhancing ability. A larger crystallite length for products obtained from native versions, compared to demineralized versions, was attributed to a formation and decomposition of a silicon carbide during graphitization of native versions. In order to examine the anisotropic and isotropic properties, nuclear-grade graphite samples obtained from Oak Ridge National Laboratory (ORNL) and commercial graphite purchased from Fluka were characterized under similar conditions as graphitized co-cokes and anthracites. These samples served as representatives of "two extremes", with ORNL samples being the isotropic end and commercial graphite being the anisotropic end. Through evaluating relationships between structural parameters, it was observed that graphitized co-cokes are situated, structurally, somewhere between the "two extremes", whereas graphitized anthracites are closer to the anisotropic end. Basically, co-cokes have a better potential than anthracites to transform to isotropic or near-isotropic graphite upon graphitization. By co-coking vacuum resid/coal instead of decant oil/coal or using 500 °C instead of 465 °C, a shift away from commercial graphite towards ORNL samples was attained. Graphitizing a semi-anthracite or demineralizing anthracites before graphitization also caused a shift towards ORNL

  8. Estimation of slagging in furnaces; Kuonaavuuden ennustaminen kivihiilen poelypoltossa

    Energy Technology Data Exchange (ETDEWEB)

    Jacobson, T.; Jaeaeskelaeinen, K.; Oeini, J.; Koskiahde, A.; Jokiniemi, J.; Pyykkoenen, J. [Imatran Voima Oy, Vantaa (Finland)

    1997-10-01

    Understanding and estimation of slagging in furnaces is essential in the design of new power plants with high steam values or in modifications like low-NO{sub x} retrofits in existing furnaces. Major slagging yields poor efficiency, difficult operation and high maintenance costs of the plant. The aim of the project is to develop a computational model for slagging in pulverized coal combustion. The model is based on Computer Controlled Scanning Electron Microscopy (CCSEM) analysis of mineral composition of the coal and physical models for behaviour of minerals inside a furnace. The analyzed mineral particles are classified to five composition classes and distributed to calculational coal particles if internal minerals of coal. The calculational coal particles and the external minerals are traced in the furnace to find out the behaviour of minerals inside the furnace. If the particle tracing indicates that the particle hits the heat transfer surface of the furnace the viscosity of the particle is determined to see if particle is sticky. The model will be implemented to 3D computational fluid dynamics based furnace simulation environment Ardemus which predicts the fluid dynamics, heat transfer and combustion in a furnace. (orig.)

  9. Heat pipes and use of heat pipes in furnace exhaust

    Science.gov (United States)

    Polcyn, Adam D.

    2010-12-28

    An array of a plurality of heat pipe are mounted in spaced relationship to one another with the hot end of the heat pipes in a heated environment, e.g. the exhaust flue of a furnace, and the cold end outside the furnace. Heat conversion equipment is connected to the cold end of the heat pipes.

  10. Utilization of steel melting electric arc furnace slag for development ...

    Indian Academy of Sciences (India)

    Administrator

    Steel melting through electric arc furnace route is gaining popularity due to its many advantages, but generates a new waste, electric arc furnace slag, which is getting accumulated and land/mine filling and road construction are the only ... is a key factor, in such constructions as breakwater blocks, foundations, shoring walls, ...

  11. Development of a cylindrical gas-fired furnace for reycling ...

    African Journals Online (AJOL)

    This study presents the development of a cylindrical gas-fired furnace, which could be used for recycling aluminum in small-scale foundries in Nigeria. The crucible, combustion chamber, suspension shaft and bearings were appropriately sized. The furnace chamber was 410 mm high and 510 mm diameter and had a ...

  12. Artificial neural networks in predicting current in electric arc furnaces

    Science.gov (United States)

    Panoiu, M.; Panoiu, C.; Iordan, A.; Ghiormez, L.

    2014-03-01

    The paper presents a study of the possibility of using artificial neural networks for the prediction of the current and the voltage of Electric Arc Furnaces. Multi-layer perceptron and radial based functions Artificial Neural Networks implemented in Matlab were used. The study is based on measured data items from an Electric Arc Furnace in an industrial plant in Romania.

  13. CHARCOAL PACKED FURNACE FOR LOW-TECH CHARRING OF BONE

    DEFF Research Database (Denmark)

    Jacobsen, P.; Dahi, Elian

    1997-01-01

    A low-tech furnace for charring of raw bone using char coal is developed and tested. The furnace consists of a standard oil drum, fitted with simple materials as available in every market in small towns in developing counties. 80 kg of raw bone and 6 kg of charcoal are used for production of 50 k...

  14. Design and Construction of Oil Fired Compact Crucible Furnace ...

    African Journals Online (AJOL)

    As a prelude to necessary industrialization, foundries are springing up in various parts of Nigeria and most of these foundries rely on oil fired furnaces in their operation. This study is aimed at developing an oil fired crucible furnace from locally sourced materials for foundries in Nigeria. In our design, a new system of fuel ...

  15. THE MOVEMENT AND MIXING OF DISPERSED MATERIALS IN ROTARY FURNACES

    Directory of Open Access Journals (Sweden)

    S. L. Rovin

    2017-01-01

    Full Text Available This article describes motion and heat and mass transfer in the layer of dispersed material in a rotary furnace. Presents the results of a comprehensive study of these processes, including pilot studies, computer modeling and simulation, which allow to optimize the design and process parameters of rotary furnaces.

  16. Dirac fermions on graphite cones

    CERN Document Server

    Osipov, V A

    2001-01-01

    The electronic structure of graphitic cones is investigated within the self-consistent field-theory model. The local and total density of states near the apex is found for cones of different opening angles. For extended electronic states, total density of states is found to vanish at the Fermi level at any opening angles more than 60 deg. In turn, for power-law localized states, normalized zero-energy modes are shown to emerge

  17. Method of operating a centrifugal plasma arc furnace

    Science.gov (United States)

    Kujawa, S.T.; Battleson, D.M.; Rademacher, E.L. Jr.; Cashell, P.V.; Filius, K.D.; Flannery, P.A.; Whitworth, C.G.

    1998-03-24

    A centrifugal plasma arc furnace is used to vitrify contaminated soils and other waste materials. An assessment of the characteristics of the waste is performed prior to introducing the waste into the furnace. Based on the assessment, a predetermined amount of iron is added to each batch of waste. The waste is melted in an oxidizing atmosphere into a slag. The added iron is oxidized into Fe{sub 3}O{sub 4}. Time of exposure to oxygen is controlled so that the iron does not oxidize into Fe{sub 2}O{sub 3}. Slag in the furnace remains relatively non-viscous and consequently it pours out of the furnace readily. Cooled and solidified slag produced by the furnace is very resistant to groundwater leaching. The slag can be safely buried in the earth without fear of contaminating groundwater. 3 figs.

  18. Considerations for Scale-Up of Ferronickel Electric Smelting Furnaces

    Science.gov (United States)

    Hundermark, R. J.; Nelson, L. R.

    2017-02-01

    In ferronickel smelting, the selective carbothermic reduction of calcined nickel laterite ores in large electric furnaces yields a crude ferronickel product. The optimal process for nickel laterite smelting requires a fine balance between the metallurgical requirements of the process (feed composition, nickel recovery, energy consumption, product quality) and the capabilities of the feeding, tapping and off-gas systems, and especially of the furnace crucible and electrical system. The scale-up of nickel laterite smelting operations over the last 50 years has seen a tenfold increase in furnace power input. Furnace operations within the industry are examined to identify common trends and some new metrics are proposed which incorporate the combination of electrode power densities and the impact of alloy nickel grade on gas generation rates, and hence local electrode gas fluxes, which may impact on future scale-up of ferronickel furnaces.

  19. Technology evaluation report of Retech, Inc., Plasma Centrifugal Furnace, volume 1

    Science.gov (United States)

    1992-07-01

    A demonstration of the Retech, Inc. Plasma Centrifugal Furnace (PCF) was conducted under the Superfund Innovative Technology Evaluation (SITE) Program at the Department of Energy's (DOE's) Component Development and Integration Facility in Butte, Montana. The furnace uses heat generated from a plasma arc to melt and vitrify solid feed material. The feed soil was a mixture of Silver Bow Creek soil and 10 percent by weight No. 2 diesel oil, spiked to provide 28,000 ppm zinc oxide and 1000 ppm hexichlorobenzene in the soil/oil mixture. Pre-treatment soil and scrubber liquor/makeup sampling was performed to characterize the material inputs to the process. Following treatment, the vitrified soil, scrubber liquor, and stack gas were sampled to determine the technology's suitability for use in destroying and immobilizing contaminants in the test soil. The results from the test were used to draw conclusions on the technology. The conclusions derived from the test results are presented.

  20. Environmentally benign graphite intercalation compound composition for exfoliated graphite, flexible graphite, and nano-scaled graphene platelets

    Science.gov (United States)

    Zhamu, Aruna; Jang, Bor Z.

    2014-06-17

    A carboxylic-intercalated graphite compound composition for the production of exfoliated graphite, flexible graphite, or nano-scaled graphene platelets. The composition comprises a layered graphite with interlayer spaces or interstices and a carboxylic acid residing in at least one of the interstices, wherein the composition is prepared by a chemical oxidation reaction which uses a combination of a carboxylic acid and hydrogen peroxide as an intercalate source. Alternatively, the composition may be prepared by an electrochemical reaction, which uses a carboxylic acid as both an electrolyte and an intercalate source. Exfoliation of the invented composition does not release undesirable chemical contaminants into air or drainage.

  1. Electrochemical Ultracapacitors Using Graphitic Nanostacks

    Science.gov (United States)

    Marotta, Christopher

    2012-01-01

    Electrochemical ultracapacitors (ECs) have been developed using graphitic nanostacks as the electrode material. The advantages of this technology will be the reduction of device size due to superior power densities and relative powers compared to traditional activated carbon electrodes. External testing showed that these materials display reduced discharge response times compared to state-of-the-art materials. Such applications are advantageous for pulsed power applications such as burst communications (satellites, cell phones), electromechanical actuators, and battery load leveling in electric vehicles. These carbon nanostructures are highly conductive and offer an ordered mesopore network. These attributes will provide more complete electrolyte wetting, and faster release of stored charge compared to activated carbon. Electrochemical capacitor (EC) electrode materials were developed using commercially available nanomaterials and modifying them to exploit their energy storage properties. These materials would be an improvement over current ECs that employ activated carbon as the electrode material. Commercially available graphite nanofibers (GNFs) are used as precursor materials for the synthesis of graphitic nanostacks (GNSs). These materials offer much greater surface area than graphite flakes. Additionally, these materials offer a superior electrical conductivity and a greater average pore size compared to activated carbon electrodes. The state of the art in EC development uses activated carbon (AC) as the electrode material. AC has a high surface area, but its small average pore size inhibits electrolyte ingress/egress. Additionally, AC has a higher resistivity, which generates parasitic heating in high-power applications. This work focuses on fabricating EC from carbon that has a very different structure by increasing the surface area of the GNF by intercalation or exfoliation of the graphitic basal planes. Additionally, various functionalities to the GNS

  2. Electron paramagnetic resonance study of nanostructured graphite

    Science.gov (United States)

    Kausteklis, Jonas; Cevc, Pavel; Arčon, Denis; Nasi, Lucia; Pontiroli, Daniele; Mazzani, Marcello; Riccò, Mauro

    2011-09-01

    We report on a systematic temperature-dependent x-band electron paramagnetic resonance (EPR) study of nanosized graphite particles prepared by ball milling. In as-prepared samples a very intense and sharp EPR resonance at g=2.0035 has been measured. The EPR line width shows a Korringa-like linear temperature dependence arising due to the coexistence and strong exchange coupling of itinerant and localized edge states. With a prolonged aging in inert atmosphere, changes in the EPR signal suggest gradual structural reconstruction where the localized edge states dominate the EPR signal. In this case the EPR spin susceptibility shows a maximum at ≈23K indicating the development of antiferromagnetic correlations as expected for the graphene lattice with a bipartite symmetry.

  3. STS-47 MS Davis uses SLJ Rack 8 continuous heating furnace (CHF) on OV-105

    Science.gov (United States)

    1992-01-01

    STS-47 Mission Specialist (MS) N. Jan Davis, wearing gloves, conducts experiment M13, Fabrication of Si-As-Te:Ni Ternary Amorphous Semiconductor in Microgravity, using the continuous heating furnace (CHF) located in the Spacelab Japan (SLJ) module on Rack 8 - NASDA Material Sciences. CHF provided temperatures up to 1,300 degrees Celsius and rapid cooling to two sets of samples concurrently. This was one of the many experiments designed and monitored by Japan's National Space Development Agency (NASDA).

  4. Effect of alkaline elements on the reactivity, strength and structural properties of blast furnace cokes

    OpenAIRE

    A. Bhattacharyya; J. Schenk; G. Rantitsch; C. Thaler; H. Stocker

    2015-01-01

    The present study concerns itself on the adverse effects of alkaline elements like sodium and potassium on blast furnace cokes. To achieve a deeper insight on the effects of alkaline elements on coke reactivity and strength, industrial coke samples impregnated with different alkaline species in various amounts have been tested under standard conditions to find out their Coke Reactivity Index (CRI) and Coke Strength after Reaction (CSR) values. Scanning electron microscopy, petrographic and Ra...

  5. Temperature-programmable furnace for ashing of foods in trace metal analysis.

    Science.gov (United States)

    Holak, W

    1977-01-01

    The use of programmable furnace in preparing samples for determining cadmium, lead, copper, and zinc by differential pulse anodic stripping voltammetry or atomic absorption spectrophotometry is convenient and time-saving. Recovery data for these 4 metals in various foods (tuna, sardines, and milk) were 93-96% for 0.01-1 ppm cadmium, 96-114% for 0.05-5 ppm lead, 100-108% for 2-10 ppm copper, and 97% for 10 ppm zinc.

  6. Determination of Zinc Ions in Environmental Samples by Dispersive Liquid- Liquid Micro Extraction and Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    F. Arabi

    2012-11-01

    Full Text Available In this work preconcentration of the Zn ions was investigated in water sample by Dispersive liquid- liquid micro extraction (DLLME using chloroform as an extraction solvent, methanol as a disperser solvent and 8-Hydroxyquinoline as a chelating agent. The determination of extracted ions was done by graphite furnace atomic absorption spectrometry. The influence of various analytical parameters including pH, extraction and disperser solvent type and volume and concentration of the chelating agent on the extraction efficiency of analyses was investigated. After extraction, the enrichment factor was 26 and the detection limit of the method was 0.0033 µg l-1 and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Zn were 7.41%. 

  7. Chitosan: a green carbon source for the synthesis of graphitic nanocarbon, tungsten carbide and graphitic nanocarbon/tungsten carbide composites

    Energy Technology Data Exchange (ETDEWEB)

    Wang Baoli; Tian Chuigui; Wang Lei; Wang Ruihong; Fu Honggang, E-mail: fuhg@vip.sina.com [Key Laboratory of Functional Inorganic Material Chemistry, Ministry of Education, Heilongjiang University, Harbin 150080 (China)

    2010-01-15

    In this paper, a simple approach was proposed to fabricate graphitic carbon nanocapsules, tungsten carbide and tungsten carbides/graphitic carbon composites by using chitosan, a green and renewable biopolymer, as a carbon source. The route includes, first, fabrication of the precursors that consist of chitosan coordinated with a certain metal ion (or metal complex anion) followed by carbonizing the precursors under N{sub 2} atmosphere. The composition of the final products could be regulated by changing the type and ratio of the metal source (cations or complex anions) combined with the chitosan in the precursors. The experimental results showed that uniform carbon nanocapsules could be obtained when Ni{sup 2+} was introducing in the precursors, while incorporating [PW{sub 12}O{sub 40}]{sup 3-} (PW{sub 12}) with chitosan led to the formation of WC nanoparticles. As the Ni{sup 2+} and PW{sub 12} are simultaneously coordinated with chitosan, the composites of tungsten carbide/graphitic carbon were successfully produced. Transmission electron microscopy (TEM) analysis revealed that the graphitic carbon nanocapsules are about 45 nm in diameter; uniform WC nanoparticles with a average size of 40 nm are observed. Moreover, the particle size of WC in the tungsten carbide/graphitic carbon composite is about 10 nm, which is smaller than that of the pure WC particles. Furthermore, the performance of the sample-loaded Pt nanoparticles for methanol electro-oxidation was studied in detail. The results indicated that the samples could act as good carriers for Pt in the methanol electro-oxidation reaction with high effectivity and improved stability.

  8. Graphite Black shale of Vendas de Ceira, Coimbra, Portugal

    Science.gov (United States)

    Quinta-Ferreira, Mário; Silva, Daniela; Coelho, Nuno; Gomes, Ruben; Santos, Ana; Piedade, Aldina

    2017-04-01

    The graphite black shale of Vendas de Ceira located in south of Coimbra (Portugal), caused serious instability problems in recent road excavation slopes. The problems increased with the rain, transforming shales into a dark mud that acquires a metallic hue when dried. The black shales are attributed to the Devonian or eventually, to the Silurian. At the base of the slope is observed graphite black shale and on the topbrown schist. Samples were collected during the slope excavation works. Undisturbed and less altered materials were selected. Further, sampling was made difficult as the graphite shale was covered by a thick layer of reinforced concrete, which was used to stabilize the excavated surfaces. The mineralogy is mainly constituted by quartz, muscovite, ilite, ilmenite and feldspar without the presence of expansive minerals. The organic matter content is 0.3 to 0.4%. The durability evaluated by the Slake Durability Test varies from very low (Id2 of 6% for sample A) to high (98% for sample C). The grain size distribution of the shale particles, was determined after disaggregation with water, which allowed verifying that sample A has 37% of fines (5% of clay and 32% of silt) and 63% of sand, while sample C has only 14% of fines (2% clay and 12% silt) and 86% sand, showing that the decrease in particle size contributes to reduce durability. The unconfined linear expansion confirms the higher expandability (13.4%) for sample A, reducing to 12.1% for sample B and 10.5% for sample C. Due the shale material degradated with water, mercury porosimetry was used. While the dry weight of the three samples does not change significantly, around 26 kN/m3, the porosity is much higher in sample A with 7.9% of pores, reducing to 1.4% in sample C. The pores size vary between 0.06 to 0.26 microns, does not seem to have any significant influence in the shale behaviour. In order to have a comparison term, a porosity test was carried out on the low weatherable brown shale, which is

  9. Low temperature vapor phase digestion of graphite

    Energy Technology Data Exchange (ETDEWEB)

    Pierce, Robert A.

    2017-04-18

    A method for digestion and gasification of graphite for removal from an underlying surface is described. The method can be utilized to remove graphite remnants of a formation process from the formed metal piece in a cleaning process. The method can be particularly beneficial in cleaning castings formed with graphite molding materials. The method can utilize vaporous nitric acid (HNO.sub.3) or vaporous HNO.sub.3 with air/oxygen to digest the graphite at conditions that can avoid damage to the underlying surface.

  10. AC induction field heating of graphite foam

    Science.gov (United States)

    Klett, James W.; Rios, Orlando; Kisner, Roger

    2017-08-22

    A magneto-energy apparatus includes an electromagnetic field source for generating a time-varying electromagnetic field. A graphite foam conductor is disposed within the electromagnetic field. The graphite foam when exposed to the time-varying electromagnetic field conducts an induced electric current, the electric current heating the graphite foam. An energy conversion device utilizes heat energy from the heated graphite foam to perform a heat energy consuming function. A device for heating a fluid and a method of converting energy are also disclosed.

  11. The Fracture Toughness of Nuclear Graphites Grades

    Energy Technology Data Exchange (ETDEWEB)

    Burchell, Timothy D. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Erdman, III, Donald L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Lowden, Rick R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Hunter, James A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Hannel, Cara C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-04-01

    New measurements of graphite mode I critical stress intensity factor, KIc (commonly referred to as the fracture toughness) and the mode II critical shear stress intensity, KIIc, are reported and compared with prior data for KIc and KIIc. The new data are for graphite grades PCEA, IG-110 and 2114. Variations of KIc and acoustic emission (AE) data with graphite texture are reported and discussed. The Codes and Standards applications of fracture toughness, KIc, data are also discussed. A specified minimum value for nuclear graphite KIc is recommended.

  12. DC Electric Arc Furnace Application for Production of Nickel-Boron Master Alloys

    Science.gov (United States)

    Alkan, Murat; Tasyürek, Kerem Can; Bugdayci, Mehmet; Turan, Ahmet; Yücel, Onuralp

    2017-09-01

    In this study, nickel-boron (Ni-B) alloys were produced via a carbothermic reduction starting from boric acid (H3BO3) with high-purity nickel oxide (NiO), charcoal, and wood chips in a direct current arc furnace. In electric arc furnace experiments, different starting mixtures were used, and their effects on the chemical compositions of the final Ni-B alloys were investigated. After the reduction and melting stages, Ni-B alloys were obtained by tapping from the bottom of the furnace. The samples from the designated areas were also taken and analyzed. The chemical composition of the final alloys and selected samples were measured with wet chemical analysis. The Ni-B alloys had a composition of up to 14.82 mass% B. The phase contents of the final alloys and selected samples were measured using x-ray diffraction (XRD). The XRD data helped predict possible reactions and reaction mechanisms. The material and energy balance calculations were made via the XRD Rietveld and chemical compositions. Nickel boride phases started to form 600 mm below the surface. The targeted NiB phase was detected at the tapping zone of the crucible (850-900 mm depth). The energy consumption was 1.84-4.29 kWh/kg, and the electrode consumption was 10-12 g/kg of raw material charged.

  13. An update on blast furnace granular coal injection

    Energy Technology Data Exchange (ETDEWEB)

    Hill, D.G. [Bethlehem Steel Corp., Burns Harbor, IN (United States); Strayer, T.J.; Bouman, R.W. [Bethlehem Steel Corp., PA (United States)

    1997-12-31

    A blast furnace coal injection system has been constructed and is being used on the furnace at the Burns Harbor Division of Bethlehem Steel. The injection system was designed to deliver both granular (coarse) and pulverized (fine) coal. Construction was completed on schedule in early 1995. Coal injection rates on the two Burns Harbor furnaces were increased throughout 1995 and was over 200 lbs/ton on C furnace in September. The injection rate on C furnace reached 270 lbs/ton by mid-1996. A comparison of high volatile and low volatile coals as injectants shows that low volatile coal replaces more coke and results in a better blast furnace operation. The replacement ratio with low volatile coal is 0.96 lbs coke per pound of coal. A major conclusion of the work to date is that granular coal injection performs very well in large blast furnaces. Future testing will include a processed sub-bituminous coal, a high ash coal and a direct comparison of granular versus pulverized coal injection.

  14. Resistance heated melting and holding furnaces for aluminium casting

    Energy Technology Data Exchange (ETDEWEB)

    Atkins, R.

    1989-02-01

    Resistance heated furnaces are ideal for holding and melter/holding applications in aluminium foundries. Electric resistance bale out furnaces can be fed with liquid metal and used as holding furnaces. They are also capable of melting at rates of 150/160 kg per hour at 720C. Improvements in element material have resulted in designs capable of maximum melt rates approaching that of fuel fired furnaces. A well proven design is available utilising semi-embedded elements in 2 versions to provide minimum energy consumption at lowest capital cost. A recent development is element panels produced by a new technique and using different materials which means the elements can be fully enclosed without any loss of performance. For larger aluminium pressure diecasting with substantial bulk melting facilities, insulated box furnaces have proved to be very attractive for holding metal at the diecasting machine. Electric immersion furnaces are also beginning to be used. These have the advantage of high efficiency and improved temperature control. The article concludes by discussing the implementation of energy management systems in conjunction with electric melting, and the introduction of electric ladles for keeping aluminium hot when transferring it from bulk furnaces.

  15. Mesoproterozoic graphite deposits, New Jersey Highlands: Geologic and stable isotopic evidence for possible algal origins

    Science.gov (United States)

    Volkert, R.A.

    2000-01-01

    Graphite deposits of Mesoproterozoic age are locally abundant in the eastern New Jersey Highlands, where they are hosted by sulphidic biotite-quartz-feldspar gneiss, metaquartzite, and anatectic pegmatite. Gneiss and metaquartzite represent a shallow marine shelf sequence of locally organic-rich sand and mud. Graphite from massive deposits within metaquartzite yielded ??13C values of -26 ?? 2??? (1??), and graphite from massive deposits within biotite-quartz-feldspar gneiss yielded ??13C values of -23 ??4???. Disseminated graphite from biotite-quartz-feldspar gneiss country rock was -22 ??3???, indistinguishable from the massive deposits hosted by the same lithology. Anatectic pegmatite is graphitic only where generated from graphite-bearing host rocks; one sample gave a ??13C value of -15???. The ??34S values of trace pyrrhotite are uniform within individual deposits, but vary from 0 to 9??? from one deposit to another. Apart from pegmatitic occurrences, evidence is lacking for long-range mobilization of carbon during Grenvillian orogenesis or post-Grenvillian tectonism. The field, petrographic, and isotope data suggest that massive graphite was formed by granulite-facies metamorphism of Proterozoic accumulations of sedimentary organic matter, possibly algal mats. Preservation of these accumulations in the sedimentary environment requires anoxic basin waters or rapid burial. Anoxia would also favour the accumulation of dissolved ferrous iron in basin waters, which may explain some of the metasediment-hosted massive magnetite deposits in the New Jersey Highlands. ?? 2000 NRC.

  16. The relationship between microstructure and oxidation effects of selected IG- and NBG-grade nuclear graphites

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Wei-Hao; Tsai, Shuo-Cheng; Yang, Chia-Wei [Department of Engineering and System Science, National Tsing-Hua University, Hsinchu 30013, Taiwan (China); Kai, Ji-Jung, E-mail: x3heat@gmail.com [Department of Engineering and System Science, National Tsing-Hua University, Hsinchu 30013, Taiwan (China); Institute of Nuclear Engineering and Science, National Tsing-Hua University, Hsinchu 30013, Taiwan (China)

    2014-11-15

    This study consists of three main parts. The first part characterizes IG- and NBG-grade nuclear graphites (IG-110, IG-430, NBG-18, and NBG-17) in terms of the size and shape of filler particles and how the forming method affects the pore distribution. The second part presents an experimental investigation of nuclear graphite oxidation at temperatures ranging from 700 to 1100 °C in air and correlates this with the theory of active sites on graphite. Mercury porosimetry is used to quantify the pore structure development at various temperatures. X-ray diffraction analysis of selected graphites is conducted to determine the crystallographic parameters. Results of mercury porosimetry and scanning electron microscopy images are correlated with the theory of active sites on graphite in order to demonstrate the relationship between pore distribution and active sites. The third part of the study presents two experiments. The first experiment considers the effects of size of samples with the same aspect ratio and the other considers actual-sized fuel pellets and graphite sleeves to evaluate the degradation of graphite components in an air-ingress scenario.

  17. Anode performance of boron-doped graphites prepared from shot and sponge cokes

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Tao; Luo, Ruiying [School of Science, Beihang University, Beijing 100083 (China); Yoon, Seong-Ho; Mochida, Isao [Institute for Materials Chemistry and Engineering, Kyushu University, Kasuga, Fukuoka 816-8580 (Japan)

    2010-03-15

    The structures and anode performances of graphitized pristine and boron-doped shot and sponge cokes have been comparatively studied by means of scanning electron microscope (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and galvanostatic measurement. The results show that high degree of graphitization can be obtained by the substituted boron atom in the carbon lattice, and boron in the resultant boron-doped graphites mainly exist in the form of boron carbide and boron substituted in the carbon lattice. Both of boron-doped graphites from shot and sponge cokes obtain discharge capacity of 350 mAh g{sup -1} and coulombic efficiency above 90%. Apart from commonly observed discharge plateau for graphite, boron-doped samples in this study also show a small plateau at ca. 0.06 V. This phenomenon can be explained that Li ion stores in the site to be void-like spaces that are produced by ''molecular bridging'' between the edge sites of graphene layer stack with a release of boron atoms substituted at the edge of graphene layer. The effect of the amount of boron dopant and graphitization temperature on the anode performance of boron-doped graphite are also investigated in this paper. (author)

  18. Anode performance of boron-doped graphites prepared from shot and sponge cokes

    Science.gov (United States)

    Liu, Tao; Luo, Ruiying; Yoon, Seong-Ho; Mochida, Isao

    The structures and anode performances of graphitized pristine and boron-doped shot and sponge cokes have been comparatively studied by means of scanning electron microscope (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and galvanostatic measurement. The results show that high degree of graphitization can be obtained by the substituted boron atom in the carbon lattice, and boron in the resultant boron-doped graphites mainly exist in the form of boron carbide and boron substituted in the carbon lattice. Both of boron-doped graphites from shot and sponge cokes obtain discharge capacity of 350 mAh g -1 and coulombic efficiency above 90%. Apart from commonly observed discharge plateau for graphite, boron-doped samples in this study also show a small plateau at ca. 0.06 V. This phenomenon can be explained that Li ion stores in the site to be void-like spaces that are produced by "molecular bridging" between the edge sites of graphene layer stack with a release of boron atoms substituted at the edge of graphene layer. The effect of the amount of boron dopant and graphitization temperature on the anode performance of boron-doped graphite are also investigated in this paper.

  19. Low-Cost Graphite-Based Free Chlorine Sensor.

    Science.gov (United States)

    Pan, Si; Deen, M Jamal; Ghosh, Raja

    2015-11-03

    Pencil lead was used to fabricate a graphite-based electrode for sensing applications. Its surface was electrochemically modified using ammonium carbamate to make it suitable for sensing free chlorine in water samples. Chlorine is widely used as a disinfectant in the water industry, and the residual free chlorine concentration in water distributed to the consumers must be lower than that stipulated by regulatory bodies. The graphite-based amperometric sensor gave a selective and linear response to free chlorine in the relevant concentration range and no response to commonly interfering ions. It was evaluated further for storage stability, response time, and hysteresis. This sensor is being proposed as a low-cost device for determining free chlorine in water samples. Its ease-of-use, limitations, and feasibility for mass-production and application is discussed.

  20. Carbon transfer from magnesia-graphite ladle refractories to ultra-low carbon steel

    Science.gov (United States)

    Russo, Andrew Arthur

    Ultra-low carbon steels are utilized in processes which require maximum ductility. Increases in interstitial carbon lower the ductility of steel; therefore, it is important to examine possible sources of carbon. The refractory ladle lining is one such source. Ladle refractories often contain graphite for its desirable thermal shock and slag corrosion resistance. This graphite is a possible source of carbon increase in ultra-low carbon steels. The goal of this research is to understand and evaluate the mechanisms by which carbon transfers to ultra-low carbon steel from magnesia-graphite ladle refractory. Laboratory dip tests were performed in a vacuum induction furnace under an argon atmosphere to investigate these mechanisms. Commercial ladle refractories with carbon contents between 4-12 wt% were used to investigate the effect of refractory carbon content. Slag-free dip tests and slag-containing dip tests with varying MgO concentrations were performed to investigate the influence of slag. Carbon transfer to the steel was controlled by steel penetrating into the refractory and dissolving carbon in dip tests where no slag was present. The rate limiting step for this mechanism is convective mass transport of carbon into the bulk steel. No detectable carbon transfer occurred in dip tests with 4 and 6 wt%C refractories without slag because no significant steel penetration occurred. Carbon transfer was controlled by the corrosion of refractory by slag in dip tests where slag was present.

  1. The technological raw material heating furnaces operation efficiency improving issue

    Science.gov (United States)

    Paramonov, A. M.

    2017-08-01

    The issue of fuel oil applying efficiency improving in the technological raw material heating furnaces by means of its combustion intensification is considered in the paper. The technical and economic optimization problem of the fuel oil heating before combustion is solved. The fuel oil heating optimal temperature defining method and algorithm analytically considering the correlation of thermal, operating parameters and discounted costs for the heating furnace were developed. The obtained optimization functionality provides the heating furnace appropriate thermal indices achievement at minimum discounted costs. The carried out research results prove the expediency of the proposed solutions using.

  2. The helium-graphite interaction

    Energy Technology Data Exchange (ETDEWEB)

    Joly, F.; Lhuillier, C.; Brami, B. (Lab. de Physique Theorique des Liquides, Univ. Pierre et Marie Curie, 75 - Paris (France))

    1992-03-15

    We propose a very simple empirical form of the helium-on-graphite potential, which reproduces the energy of the six known bound states, the experimental average distance of the {sup 4}He atom from the surface in the ground state and the correct asymptotic behaviour of the interaction. This optimized potential is used to compute the binding energy of a {sup 3}He atom on the same substrate. The agreement between the theoretical predictions and the experimental results is a check of the set of variational parameters. (orig.).

  3. Contact Angle Hysteresis on Graphene Surfaces and Hysteresis-free Behavior on Oil-infused Graphite Surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Cyuan-Jhang; Li, Yueh-Feng [Department of Chemical and Materials Engineering, National Central University, Jhongli 320, Taiwan (China); Woon, Wei-Yen [Department of Physics, National Central University, Jhongli 320, Taiwan (China); Sheng, Yu-Jane, E-mail: yjsheng@ntu.edu.tw [Department of Chemical Engineering, National Taiwan University, Taipei 106, Taiwan (China); Tsao, Heng-Kwong, E-mail: hktsao@cc.ncu.edu.tw [Department of Chemical and Materials Engineering, National Central University, Jhongli 320, Taiwan (China); Department of Physics, National Central University, Jhongli 320, Taiwan (China)

    2016-11-01

    Highlights: • Contact angle hysteresis(CAH) on four graphitic surfacesisinvestigated. • The hysteresis loopof water drops on the polished graphite sheetshowsparticularly small receding contact angle. • The significant CAH observed on CVD graphene and highly oriented pyrolytic graphite is attributed mainly to adhesion hysteresis. • An oil-infused surface of a graphite sheet is produced by imbibition of hexadecane into its porous structure. • The hysteresis-free property for water drops on such a surface is examined and quantitatively explained. - Abstract: Contact angle hysteresis (CAH) on graphitic surfaces, including chemical vapor deposition (CVD) graphene, reduced electrophoretic deposition (EPD) graphene, highly oriented pyrolytic graphite (HOPG), and polished graphite sheet, has been investigated. The hysteresis loops of water drops on the first three samples are similar but the receding contact angle is particularly small for the polished graphite sheet.The significant CAH observed on CVD graphene and HOPG associated with atom-scale roughness has to be attributed mainly to adhesion hysteresis (surface relaxation), instead of roughness or defects.The difference of the wetting behavior among those four graphitic samples has been further demonstrated by hexadecane drops. On the surface of HOPG or CVD graphene,the contact line expands continuously with time, indicating total wetting for which the contact angle does not exist and contact line pinning disappears. In contrast, on the surface of reduced EPD graphene, spontaneous spreading is halted by spikes on it and partial wetting with small contact angle (θ≈4°) is obtained. On the surface of polished graphite sheet, the superlipophilicity and porous structure are demonstrated by imbibition and capillary rise of hexadecane. Consequently, an oil-infused graphite surface can be fabricated and the ultralow CAH of water (∆θ≈2°) is achieved.

  4. Production of durable expanded perlite microspheres in a Vertical Electrical Furnace

    Science.gov (United States)

    Panagiotis, M.; Angelopoulos, P.; Taxiarchou, M.; Paspaliaris, I.

    2016-04-01

    Expanded perlite constitutes one of the most competitive insulating materials that is widely used in construction and manufacturing industry due to its unique properties combination; it is white, natural, lightweight, chemically inert, and exhibits superior insulating properties (thermal and acoustic) and fire resistance. Conventionally, perlite expansion is performed in vertical gas-fired furnaces; the conventional perlite expansion process has certain disadvantages which affect expanded products quality, thus limiting their performance and range of applications. In order to overcome the drawbacks of the conventional expansion technique, a new perlite expansion process has been designed based on a vertical electrical furnace (VEF). In the current study, fine perlite samples (-150 μm) from Milos Island, Greece, were expansed in the novel VEF and a conventional gas-fired furnace with the aim to evaluate and compare the main physical properties of the expanded products. The novel expanded perlite particles were characterised by superior properties, namely increased compression strength, competitive water and oil absorption capability, size homogeneity, spherical shape and decreased surface porosity in comparison to conventionally expanded samples.

  5. Impact of muffle furnace preparation on the results of crystalline silica analysis.

    Science.gov (United States)

    Lee, R J; Van Orden, D R; Cox, L A; Arlauckas, S; Kautz, R J

    2016-10-01

    A prior report demonstrated an unacceptably low level of accuracy in silica analytical testing, with a general negative bias (i.e., underreporting) although other inaccuracies included false-positive results when analyzing blank filters. The possible bias may have been due to the loss of sample during shipping and or sample preparation. We report on a follow-up study that was designed to mimic the original study, but in which sources of variability were evaluated. We found no effect on silica recoveries due to shipping and confirmed the prior study results that the muffle furnace ashing process led to low overall recoveries (49-104%), depending on the adherence to the recommended preparation method. Plasma ashing recoveries ranged from 89 to 108%. Our results suggest that muffle-furnace ashing using a crucible should be restricted. More broadly, however, muffle-furnace ashing is only one source of analytical error that contributes to the relatively poor overall performance revealed by Cox et al. Whatever the case, OSHA should ensure that its proposed requirements to improve laboratory performance will actually lead to the discovery and correction of all major sources of error by participating laboratories. This is particularly important in light of OSHA's proposed reduction in the PEL and action level proposed by OSHA. Copyright © 2016 Elsevier Inc. All rights reserved.

  6. Studies on POM/graphite/Ekonol composites

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 26; Issue 6. Studies on POM/graphite/Ekonol ... POM/graphite/Ekonol composites were prepared by the Torque Rheometer mixing and compression molding, and their hardness, compressive and impact strengths have been tested. The tribology behaviour was also ...

  7. Tire containing thermally exfoliated graphite oxide

    Science.gov (United States)

    Prud'homme, Robert K. (Inventor); Aksay, Ilhan A. (Inventor)

    2011-01-01

    A tire, tire lining or inner tube, containing a polymer composite, made of at least one rubber and/or at least one elastomer and a modified graphite oxide material, which is a thermally exfoliated graphite oxide with a surface area of from about 300 sq m/g to 2600 sq m/g.

  8. Inhibition of Oxidation in Nuclear Graphite

    Energy Technology Data Exchange (ETDEWEB)

    Phil Winston; James W. Sterbentz; William E. Windes

    2013-10-01

    Graphite is a fundamental material of high temperature gas cooled nuclear reactors, providing both structure and neutron moderation. Its high thermal conductivity, chemical inertness, thermal heat capacity, and high thermal structural stability under normal and off normal conditions contribute to the inherent safety of these reactor designs. One of the primary safety issues for a high temperature graphite reactor core is the possibility of rapid oxidation of the carbon structure during an off normal design basis event where an oxidizing atmosphere (air ingress) can be introduced to the hot core. Although the current Generation IV high temperature reactor designs attempt to mitigate any damage caused by a postualed air ingress event, the use of graphite components that inhibit oxidation is a logical step to increase the safety of these reactors. Recent experimental studies of graphite containing between 5.5 and 7 wt% boron carbide (B4C) indicate that oxidation is dramatically reduced even at prolonged exposures at temperatures up to 900°C. The proposed addition of B4C to graphite components in the nuclear core would necessarily be enriched in B-11 isotope in order to minimize B-10 neutron absorption and graphite swelling. The enriched boron can be added to the graphite during billet fabrication. Experimental oxidation rate results and potential applications for borated graphite in nuclear reactor components will be discussed.

  9. Hydrogen storage in graphite nanofibers

    Energy Technology Data Exchange (ETDEWEB)

    Park, C.; Tan, C.D.; Hidalgo, R.; Baker, R.T.K.; Rodriguez, N.M. [Northeastern Univ., Boston, MA (United States). Chemistry Dept.

    1998-08-01

    Graphite nanofibers (GNF) are a type of material that is produced by the decomposition of carbon containing gases over metal catalyst particles at temperatures around 600 C. These molecularly engineered structures consist of graphene sheets perfectly arranged in a parallel, perpendicular or at angle orientation with respect to the fiber axis. The most important feature of the material is that only edges are exposed. Such an arrangement imparts the material with unique properties for gas adsorption because the evenly separated layers constitute the most ordered set of nanopores that can accommodate an adsorbate in the most efficient manner. In addition, the non-rigid pore walls can also expand so as to accommodate hydrogen in a multilayer conformation. Of the many varieties of structures that can be produced the authors have discovered that when gram quantities of a selected number of GNF are exposed to hydrogen at pressures of {approximately} 2,000 psi, they are capable of adsorbing and storing up to 40 wt% of hydrogen. It is believed that a strong interaction is established between hydrogen and the delocalized p-electrons present in the graphite layers and therefore a new type of chemistry is occurring within these confined structures.

  10. CMOS Thermal Ox and Diffusion Furnace: Tystar Tytan 2000

    Data.gov (United States)

    Federal Laboratory Consortium — Description:CORAL Names: CMOS Wet Ox, CMOS Dry Ox, Boron Doping (P-type), Phos. Doping (N-Type)This four-stack furnace bank is used for the thermal growth of silicon...

  11. Innovation in electric arc furnaces scientific basis for selection

    CERN Document Server

    Toulouevski, Yuri N

    2013-01-01

    This book equips a reader with knowledge necessary for critical analysis of  innovations in electric arc furnaces and helps to select the most effective ones and for their successful implementation. The book also covers general issues related to history of development, current state and prospects of steelmaking in Electric Arc Furnaces. Therefore, it can be useful for everybody who studies metallurgy, including students of colleges and universities. The modern concepts of mechanisms of Arc Furnace processes are are discussed in the book at the level sufficient to solve practical problems: To help readers lacking knowledge required in the field of heat transfer as well as hydro-gas dynamics, it contains several chapters which provide the required minimum of information in these fields of science. In order to better assess different innovations, the book describes experience of the application of similar innovations in open-hearth furnaces and oxygen converters. Some promising ideas on key issues regarding int...

  12. Silica crown refractory corrosion in glass melting furnaces

    National Research Council Canada - National Science Library

    Balandis A; Nizeviciene D

    2011-01-01

    ... of glass furnaces, when the rate of corrosion of crowns were about 2 times greater. The change of these parameters, the chemical composition and formation of the microcracks in the used silica refractories material were studied...

  13. Alloying and Casting Furnace for Shape Memory Alloys Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The concept in the proposed project is to create a melting, alloying and casting furnace for the processing titanium based SMA using cold crucible techniques. The...

  14. Design considerations for solar furnace focal zone apparatus

    Energy Technology Data Exchange (ETDEWEB)

    Sievers, R.H. Jr.; Knasel, T.M.; McDonnell, M.; Gordon, B.; Woods, S.; Malinowski, R.

    1981-01-01

    Science Applications, Inc. has used the principal solar furnaces in conjunction with its study of the effect of high thermal fluxes and fluences on soil surfaces for the Defense Nuclear Agency. Apparatus to perform these tests has evolved from tests on the furnaces at the White Sands Missile Range, Georgia Institute of Technology in Atlanta; Centre National de Recherche Scientifique in Font Romeu, France; and Kirtland AFB, NM over the past 6 years. The apparatus is still evolving as it is adapted to additional furnaces and to obtain a greater variety of data. The evolution of the apparatus is traced to illustrate the interaction of experiment objectives; furnace capabilities, configuration, and support; apparatus design; data collection; and response to lessons learned.

  15. Hopewell Furnace NHS Small Scale Features (Linear Features)

    Data.gov (United States)

    National Park Service, Department of the Interior — This shapefile represents the linear small scale features found at Hopewell Furnace National Historic Site based on the Cultural Landscape Report completed in...

  16. DEVELOPMENT OF A FURNACE TO FABRICATE SILICON SOLAR CELLS

    Directory of Open Access Journals (Sweden)

    Sérgio Boscato Garcia

    2012-06-01

    Full Text Available Solar cell world market had an exponential growth in the last decade and nowadays it continues in expansion. To produce solar cells, dopants need to be introduced into the crystalline silicon wafer in order to form the pn junction. This process is carried out in diffusion furnaces. The aim of this paper is to present the development of a compact diffusion furnace to process up to 156 mm × 156 mm silicon wafers and to operate at temperature up to 1100°C. The furnace is automated and it is constituted by a heating system with three zones and systems to introduce the wafers inside the furnace as well as to control of gas flows. This equipment is the first one developed in Brazil to promote impurity diffusions in order to produce silicon solar cells and it was manufactured jointly with a Brazilian company.

  17. Optimization of the melting process of electrical furnaces in drenas

    Directory of Open Access Journals (Sweden)

    A. Haxhiaj

    2012-10-01

    Full Text Available The weight, composition and loads are the main parameters of the melting process in electrical furnace. The charge is roasted in rotary furnace. Roasting of charge which consists of Drenas and Albanians ore is done at about 950°C. Also, article has the experimental analyses that modify some parameters of the production which are the reduction of quantity of limestone and the increase of quantity of quartz in the charge. The paper analysis the possibility of mixing the ore from Kosova with lateritic ore from Albania with the aim of reducing the acidity of weight which is loaded in the electrical furnace. The composition of the furnace must satisfy the ratio 1:10 of ore from Kosova and Albania.

  18. The Flexibility of Pusher Furnace Grate

    Directory of Open Access Journals (Sweden)

    Słowik J.A.

    2016-12-01

    Full Text Available The lifetime of guide grates in pusher furnaces for heat treatment could be increased by raising the flexibility of their structure through, for example, the replacement of straight ribs, parallel to the direction of grate movement, with more flexible segments. The deformability of grates with flexible segments arranged in two orientations, i.e. crosswise (perpendicular to the direction of compression and lengthwise (parallel to the direction of compression, was examined. The compression process was simulated using SolidWorks Simulation program. Relevant regression equations were also derived describing the dependence of force inducing the grate deformation by 0.25 mm ‒ modulus of grate elasticity ‒ on the number of flexible segments in established orientations. These calculations were made in Statistica and Scilab programs. It has been demonstrated that, with the same number of segments, the crosswise orientation of flexible segments increases the grate structure flexibility in a more efficient way than the lengthwise orientation. It has also been proved that a crucial effect on the grate flexibility has only the quantity and orientation of segments (crosswise / lengthwise, while the exact position of segments changes the grate flexibility by less than 1%.

  19. Investigation of radiative heat transfer in fixed bed biomass furnaces

    Energy Technology Data Exchange (ETDEWEB)

    T. Klason; X.S. Bai; M. Bahador; T.K. Nilsson; B. Sunden [Lund Institute of Technology, Lund (Sweden). Division of Fluid Mechanics

    2008-08-15

    This paper presents an investigation of the radiative heat transfer process in two fixed bed furnaces firing biomass fuels and the performance of several widely used models for calculation of radiative heat transfer in the free-room of fixed bed furnaces. The effective mean grey gas absorption coefficients are calculated using an optimised version of the exponential wide band model (EWBM) based on an optical mean beam length. Fly-ash and char particles are taken into account using Mie scattering. In the investigated updraft small-scale fixed bed furnace radiative transfer carries heat from the bed to the free-room, whereas in the cross-current bed large-scale industry furnace, radiative transfer brings heat from the hot zones in the free-room to the drying zone of the bed. Not all the investigated models can predict these heat transfer trends, and the sensitivity of results to model parameters is fairly different in the two furnaces. In the small-scale furnace, the gas absorption coefficient predicted by using different optical lengths has great impact on the predicted temperature field. In the large-scale furnaces, the predicted temperature field is less sensitive to the optical length. In both furnaces, with the same radiative properties, the low-computational-cost P1 model predicts a temperature field in the free-room similar to that by the more time consuming SLW model. In general, the radiative heat transfer rates to the fuel bed are not very sensitive to the radiative properties, but they are sensitive to the different radiative heat transfer models. For a realistic prediction of the radiative heat transfer rate to the fuel bed or to the walls, more computationally demanding models such as the FGG or SLW models should be used. 37 refs., 7 figs., 2 tabs.

  20. Modeling Fission Product Sorption in Graphite Structures

    Energy Technology Data Exchange (ETDEWEB)

    Szlufarska, Izabela [University of Wisconsin, Madison, WI (United States); Morgan, Dane [University of Wisconsin, Madison, WI (United States); Allen, Todd [University of Wisconsin, Madison, WI (United States)

    2013-04-08

    The goal of this project is to determine changes in adsorption and desorption of fission products to/from nuclear-grade graphite in response to a changing chemical environment. First, the project team will employ principle calculations and thermodynamic analysis to predict stability of fission products on graphite in the presence of structural defects commonly observed in very high- temperature reactor (VHTR) graphites. Desorption rates will be determined as a function of partial pressure of oxygen and iodine, relative humidity, and temperature. They will then carry out experimental characterization to determine the statistical distribution of structural features. This structural information will yield distributions of binding sites to be used as an input for a sorption model. Sorption isotherms calculated under this project will contribute to understanding of the physical bases of the source terms that are used in higher-level codes that model fission product transport and retention in graphite. The project will include the following tasks: Perform structural characterization of the VHTR graphite to determine crystallographic phases, defect structures and their distribution, volume fraction of coke, and amount of sp2 versus sp3 bonding. This information will be used as guidance for ab initio modeling and as input for sorptivity models; Perform ab initio calculations of binding energies to determine stability of fission products on the different sorption sites present in nuclear graphite microstructures. The project will use density functional theory (DFT) methods to calculate binding energies in vacuum and in oxidizing environments. The team will also calculate stability of iodine complexes with fission products on graphite sorption sites; Model graphite sorption isotherms to quantify concentration of fission products in graphite. The binding energies will be combined with a Langmuir isotherm statistical model to predict the sorbed concentration of fission

  1. Influence of Particle Size on Properties of Expanded Graphite

    Directory of Open Access Journals (Sweden)

    Kurajica, S

    2010-02-01

    Full Text Available Expanded graphite has been applied widely in thermal insulation, adsorption, vibration damping, gasketing, electromagnetic interference shielding etc. It is made by intercalation of natural flake graphite followed by thermal expansion. Intercalation is a process whereby an intercalant material is inserted between the graphene layers of a graphite crystal. Exfoliation, a huge unidirectional expansion of the starting intercalated flakes, occurs when the graphene layers are forced apart by the sudden decomposition and vaporization of the intercalated species by thermal shock. Along with production methodologies, such as the intercalation process and heat treatment, the raw material characteristics, especially particle size, strongly influence the properties of the final product.This report evaluates the influence of the particle size of the raw material on the intercalation and expansion processes and consequently the properties of the exfoliated graphite. Natural crystalline flake graphite with wide particle diameter distribution (between dp = 80 and 425 µm was divided into four size-range portions by sieving. Graphite was intercalated via perchloric acid, glacial acetic acid and potassium dichromate oxidation and intercalation procedure. 5.0 g of graphite, 7.0 g of perchloric acid, 4.0 g of glacial acetic acid and 2.0 g of potassium dichromate were placed in glass reactor. The mixture was stirred with n = 200 min–1 at temperature of 45 °C during 60 min. Then it was filtered and washed with distilled water until pH~6 and dried at 60 °C during 24 h. Expansion was accomplished by thermal shock at 1000 °C for 1 min. The prepared samples were characterized by means of exfoliation volume measurements, simultaneous differential thermal analysis and thermo-gravimetry (DTA/TGA, X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, BET measurements and scanning electron microscopy (SEM.X-ray diffraction indicated a change of distance

  2. Mathematical model and software for control of commissioning blast furnace

    Science.gov (United States)

    Spirin, N. A.; Onorin, O. P.; Shchipanov, K. A.; Lavrov, V. V.

    2016-09-01

    Blowing-in is a starting period of blast furnace operation after construction or major repair. The current approximation methods of blowing-in burden analysis are based on blowing-in practice of previously commissioned blast furnaces. This area is theoretically underexplored; there are no common scientifically based methods for selection of the burden composition and blast parameters. The purpose of this paper is development and scientific substantiation of the methods for selection of the burden composition and blast parameters in the blast furnace during the blowing-in period. Research methods are based on physical regularities of main processes running in the blast furnace, system analysis, and application of modern principles for development and construction of mathematical models, algorithms and software designed for automated control of complex production processes in metallurgy. As consequence of the research made by the authors the following results have been achieved: 1. A set of mathematical models for analysis of burden arrangement throughout the height of the blast furnace and for selection of optimal blast and gas dynamic parameters has been developed. 2. General principles for selection of the blowing-in burden composition and blast and gas dynamic parameters have been set up. 3. The software for the engineering and process staff of the blast furnace has been developed and introduced in the industry.

  3. Similarity of Ferrosilicon Submerged Arc Furnaces With Different Geometrical Parameters

    Directory of Open Access Journals (Sweden)

    Machulec B.

    2017-12-01

    Full Text Available In order to determine reasons of unsatisfactory production output regarding one of the 12 MVA furnaces, a comparative analysis with a furnace of higher power that showed a markedly better production output was performed. For comparison of ferrosilicon furnaces with different geometrical parameters and transformer powers, the theory of physical similarity was applied. Geometrical, electrical and thermal parameters of the reaction zones are included in the comparative analysis. For furnaces with different geometrical parameters, it is important to ensure the same temperature conditions of the reaction zones. Due to diverse mechanisms of heat generation, different criteria for determination of thermal and electrical similarity for the upper and lower reaction zones were assumed contrary to other publications. The parameter c3 (Westly was assumed the similarity criterion for the upper furnace zones where heat is generated as a result of resistive heating while the parameter J1 (Jaccard was assumed the similarity criterion for the lower furnace zones where heat is generated due to arc radiation.

  4. Characterization of steel mill electric-arc furnace dust.

    Science.gov (United States)

    Sofilić, Tahir; Rastovcan-Mioc, Alenka; Cerjan-Stefanović, Stefica; Novosel-Radović, Vjera; Jenko, Monika

    2004-06-18

    In order to make a complete characterization of electric-arc furnace (EAF) dust, as hazardous industrial waste, and to solve its permanent disposal and/or recovery, bearing in mind both the volumes formed in the Croatian steel industry and experiences of developed industrial countries, a study of its properties was undertaken. For this purpose, samples of EAF dust, taken from the regular production process in the Zeljezara Sisak Steel Mill between December 2000 and December 2001, were subjected to a series of tests. The chemical composition of EAF dust samples was investigated by means of a several different analytical methods. The results from the chemical analysis show that the approximate order of abundance of major elements in EAF dusts is as follows: Fe, Zn, Mn, Ca, Mg, Si, Pb, S, Cr, Cu, Al, C, Ni, Cd, As and Hg. Granular-metric composition of single samples was determined by applying sieve separation. Scanning electron micro-structural examination of EAF dust microstructure was performed and results indicated that all twelve EAF dusts were composed of solid spherical agglomerates with Fe, Zn, Pb, O, Si and Ca as the principal element. The investigation of grain morphology and the mineralogical composition of EAF dust were taken by combination of high resolution Auger electron spectroscopy (HR AES), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction analysis. The analysis of XPS-spectra determined the presence of zinc in the form of ZnO phase and the presence of lead in the form of PbO phase, i.e. PbSO3/PbSO4 forms. The results of the X-ray diffraction phase analysis show that the basis of the examined EAF dust samples is made of a mixture of metal oxides, silicates and sulphates. The metal concentration, anions, pH value and conductivity in water eluates was determined in order to define the influence of EAF dust on the environment.

  5. Assessing energy efficiency of electric car bottom furnaces intended for thermal energization of minerals

    Science.gov (United States)

    Nizhegorodov, A. I.

    2017-01-01

    The paper deals with a new concept of electric furnaces for roasting and thermal energization of vermiculite and other minerals with vibrational transportation of a single-layer mass under constant thermal field. The paper presents performance calculation and comparative assessment of energy data for furnaces of different modifications: flame and electric furnaces with three units, furnaces with six units and ones with series-parallel connection of units, and furnaces of new concept.

  6. Carbothermic reduction of electric arc furnace dust and calcination of waelz oxide by semi-pilot scale rotary furnace

    National Research Council Canada - National Science Library

    Morcali M.H; Yucel O; Aydin A; Derin B

    2012-01-01

    The paper gives a common outline about the known recycling techniques from electric arc furnace dusts and describes an investigation of a pyrometallurgical process for the recovery of zinc and iron...

  7. The forty years of vermicular graphite cast iron development in China (PartⅠ

    Directory of Open Access Journals (Sweden)

    CHEN Zheng-de

    2007-05-01

    Full Text Available In China, the research and development of vermicular graphite cast iron (VGCI as a new type of engineering material, were started in the same period as in other developed countries; however, its actual industrial application was even earlier. In China, the deep and intensive studies on VGCI began as early as the 1960s. According to the incomplete statistics to date, more than 600 papers on VGCI have been published by Chinese researchers and scholars at national and international conferences, and in technical journals. More than ten types of production methods and more than thirty types of treatment alloy have been studied. Formulae for calculating the critical addition of treatment alloy required to produce VGCI have been put forward, and mechanisms for explaining the formation of dross during treatment were brought forward. The casting properties, metallographic structure, mechanical and physical properties and machining performance of VGCI, as well as the relationships between them, have all been studied in detail. The Chinese Standards for VGCI and VGCI metallographic structure have been issued. In China, the primary crystallization of VGCI has been studied by many researchers and scholars. The properties of VGCI can be improved by heat treatment and addition of alloying elements enabling its applications to be further expanded. Hundreds of kinds of VGCI castings have been produced and used in vehicles, engines, mining equipment, metallurgical products serviced under alternating thermal load, machinery, hydraulic components, textile machine parts and military applications. The heaviest VGCI casting produced is 38 tons and the lightest is only 1 kg. Currently, the annual production of the VGCI in China is about 200 000 tons. The majority of castings are made from cupola iron without pre-treatment, however, they are also produced from electric furnaces and by duplex melting from cupolaelectric furnaces or blast furnace-electric furnace

  8. Experimental modelling of plasma-graphite surface interaction in ITER

    Energy Technology Data Exchange (ETDEWEB)

    Martynenko, Yu.V.; Guseva, M.I.; Gureev, V.M.; Danelyan, L.S.; Neumoin, V.E.; Petrov, V.B.; Khripunov, B.I.; Sokolov, Yu.A.; Stativkina, O.V.; Stolyarova, V.G. [Rossijskij Nauchnyj Tsentr ``Kurchatovskij Inst.``, Moscow (Russian Federation); Vasiliev, V.I.; Strunnikov, V.M. [TRINITI, Troizk (Russian Federation)

    1998-10-01

    The investigation of graphite erosion under normal operation ITER regime and disruption was performed by means of exposure of RGT graphite samples in a stationary deuterium plasma to a dose of 10{sup 22} cm{sup -2} and subsequent irradiation by power (250 MW/cm{sup 2}) pulse deuterium plasma flow imitating disruption. The stationary plasma exposure was carried out in the installation LENTA with the energy of deuterium ions being 200 eV at target temperatures of 770 C and 1150 C. The preliminary exposure in stationary plasma at temperature of physical sputtering does not essentially change the erosion due to a disruption, whereas exposure at the temperature of radiation enhanced sublimation dramatically increases the erosion due to disruption. In the latter case, the depth of erosion due to a disruption is determined by the depth of a layer with decreased strength. (orig.) 9 refs.

  9. Preparation of graphene by electrical explosion of graphite sticks.

    Science.gov (United States)

    Gao, Xin; Xu, Chunxiao; Yin, Hao; Wang, Xiaoguang; Song, Qiuzhi; Chen, Pengwan

    2017-08-03

    Graphene nanosheets were produced by electrical explosion of high-purity graphite sticks in distilled water at room temperature. The as-prepared samples were characterized by various techniques to find different forms of carbon phases, including graphite nanosheets, few-layer graphene, and especially, mono-layer graphene with good crystallinity. Delicate control of energy injection is critical for graphene nanosheet formation, whereas mono-layer graphene was produced under the charging voltage of 22.5-23.5 kV. On the basis of electrical wire explosion and our experimental results, the underlying mechanism that governs the graphene generation was carefully illustrated. This work provides a simple but innovative route for producing graphene nanosheets.

  10. TECHNOLOGICAL PECULIARITIES O F MELTING AND OUT-OF-FURNACE PROCESSING OF BALANCED STEELS IN CONDITIONS OF ELECTRIC FURNACE STEELMAKING AND CONTINUOUS CASTING

    Directory of Open Access Journals (Sweden)

    S. V. Terletski

    2007-01-01

    Full Text Available The technological peculiarities of melting and out-of-furnace processing of balanced steels in conditions of electric furnace steelmaking and continuous cast of RUP “BMZ” are considered.

  11. Effect of ash circulation in gasification melting system on concentration and leachability of lead in melting furnace fly ash.

    Science.gov (United States)

    Okada, Takashi; Suzuki, Masaru

    2013-11-30

    In some gasification-melting plants, generated melting furnace fly ash is returned back to the melting furnace for converting the ash to slag. This study investigated the effect of such ash circulation in the gasification-melting system on the concentration and leachability of lead in the melting furnace fly ash. The ash circulation in the melting process was simulated by a thermodynamic calculation, and an elemental analysis and leaching tests were performed on a melting furnace fly ash sample collected from the gasification-melting plant with the ash circulation. It was found that by the ash circulation in the gasification-melting, lead was highly concentrated in the melting furnace fly ash to the level equal to the fly ash from the ash-melting process. The thermodynamic calculation predicted that the lead volatilization by the chlorination is promoted by the ash circulation resulting in the high lead concentration. In addition, the lead extraction from the melting furnace fly ash into a NaOH solution was also enhanced by the ash circulation, and over 90% of lead in the fly ash was extracted in 5 min when using 0.5 mol l(-1) NaOH solution with L/S ratio of 10 at 100 °C. Based on the results, a combination of the gasification-melting with the ash circulation and the NaOH leaching method is proposed for the high efficient lead recovery. Copyright © 2013 Elsevier Ltd. All rights reserved.

  12. Vanadium bioavailability in soils amended with blast furnace slag

    Energy Technology Data Exchange (ETDEWEB)

    Larsson, Maja A., E-mail: maja.larsson@slu.se [Department of Soil and Environment, Swedish University of Agricultural Sciences, P.O. Box 7014, 750 07 Uppsala (Sweden); Baken, Stijn, E-mail: stijn.baken@ees.kuleuven.be [Department of Earth and Environmental Sciences, Leuven University, Kasteelpark Arenberg 20 bus 2459, 3001 Leuven (Belgium); Smolders, Erik, E-mail: erik.smolders@ees.kuleuven.be [Department of Earth and Environmental Sciences, Leuven University, Kasteelpark Arenberg 20 bus 2459, 3001 Leuven (Belgium); Cubadda, Francesco, E-mail: francesco.cubadda@iss.it [Department of Food Safety and Veterinary Public Health, Istituto Superiore di Sanità, Viale Regina Elena 299, Rome 00161 (Italy); Gustafsson, Jon Petter, E-mail: jon-petter.gustafsson@slu.se [Department of Soil and Environment, Swedish University of Agricultural Sciences, P.O. Box 7014, 750 07 Uppsala (Sweden); Division of Land and Water Resources Engineering, KTH Royal Institute of Technology, Brinellvägen 28, 100 44 Stockholm (Sweden)

    2015-10-15

    Blast furnace (BF) slags are commonly applied as soil amendments and in road fill material. In Sweden they are also naturally high in vanadium. The aim of this study was to assess the vanadium bioavailability in BF slags when applied to soil. Two soils were amended with up to 29% BF slag (containing 800 mg V kg{sup −1}) and equilibrated outdoors for 10 months before conducting a barley shoot growth assay. Additional soil samples were spiked with dissolved vanadate(V) for which assays were conducted two weeks (freshly spiked) and 10 months (aged) after spiking. The BF slag vanadium was dominated by vanadium(III) as shown by V K-edge XANES spectroscopy. In contrast, results obtained by HPLC-ICP-MS showed that vanadium(V), the most toxic vanadium species, was predominant in the soil solution. Barley shoot growth was not affected by the BF slag additions. This was likely due to limited dissolution of vanadium from the BF slag, preventing an increase of dissolved vanadium above toxic thresholds. The difference in vanadium bioavailability among treatments was explained by the vanadium concentration in the soil solution. It was concluded that the vanadium in BF slag is sparingly available. These findings should be of importance in environmental risk assessment.

  13. Emissions of dioxin and dibenzofuran from electric arc furnaces

    Directory of Open Access Journals (Sweden)

    Figueira, S. L.

    2005-06-01

    Full Text Available This paper describes work done in order to clarify the formation mechanism of highly toxic micropoUutants, such as dioxins and dibenzofurans, from electric arc furnaces used in the production of carbon steel from scrap. The study is allowing to derive relationships between the levels of airborne micropoUutants and the operational parameters of the production process so that an abatement of pollution could be achieved. By using the European standard method CEN 1948 for dioxin like compounds sampling and measurement, it was possible to determine the characteristic fingerprint of micropoUutants emitted by this particular stationary source.

    Este artículo contiene resultados del trabajo ejecutado para el esclarecimiento de los mecanismos de formación de los micropolutantes muy tóxicos, como dioxinas y dibenzofuranos, que son emitidos por los hornos de arco eléctrico utilizados en la producción de acero. Estos estudios han permitido relacionar las concentraciones de polutantes emitidos a la atmósfera con las condiciones operación del homo eléctrico. Utilizando el método normalizado CEN 1948 para captación y análisis de muestras de compuestos análogos a las dioxinas ha sido posible determinar el perfil característico de los micropolutantes emitidos por esta fuente

  14. Stabilization of electric-arc furnace dust in concrete

    Directory of Open Access Journals (Sweden)

    Carlos Alberto Caldas de Souza

    2010-12-01

    Full Text Available Electric-arc furnace dust (EAFD is a by-product of steel production and recycling. This fine-grained material contains high amounts of zinc and iron as well as significant amounts of potentially toxic elements such as lead, cadmium and chromium. Therefore, the treatment and stabilization of this industrial residue is necessary. Concrete is a well-known suitable environment for stabilization/solidification of materials which have leachable elements in need of fixation. The effect of the EAFD content on the mechanical and chemical performance of Portland cement concrete is investigated in this paper. The effect of the EAFD content on the setting time of cement slurry was also analyzed. The axial compressive strength of the concrete samples increases with the EAFD addition in the range of 10 to 20 wt. (% EAFD; also the tensile strength increases with the EAFD addition. An increase in EAFD content significantly increases the setting time of the concrete. The acetic acid leaching and water solubilization tests indicate low mobility of the potentially toxic elements from the EAFD concrete composite. The results of the immersion tests show that the addition of EAFD to the concrete seems to reduce chloride penetration, which may help prevent pitting corrosion in reinforced concrete.

  15. Application of thermospray flame furnace atomic absorption spectrometry for investigation of silver nanoparticles.

    Science.gov (United States)

    Sirirat, Natnicha; Tetbuntad, Kornrawee; Siripinyanond, Atitaya

    2017-03-01

    Thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was applied to investigate the time-dependent absorption peak profile of various forms of silver. The thermospray flame furnace was set up with a 10-cm-long nickel tube with six holes, each 2.0 mm in diameter, to allow the flame to enter, and this nickel tube acted as a furnace. A sample of 300 μL was introduced into this furnace by use of water as a carrier at a flow rate of 0.5 mL min-1 through the ceramic capillary (0.5-mm inner diameter and 2.0-mm outer diameter), which was inserted into the front hole of the nickel tube. The system was applied to examine atomization behaviors of silver nanoparticles (AgNPs) with particle sizes ranging from 10 to 100 nm. The atomization rate of AgNPs was faster than that of the dissolved silver ion. With increased amount of silver, the decay time observed from the time-dependent absorption peak profile was shortened in the case of dissolved silver ion, but it was increased in the case of AgNPs. With the particle size ranging from 10 to 100 nm, the detection sensitivity was indirectly proportional to the particle size, suggesting that TS-FF-AAS may offer insights into the particle size of AgNPs provided that the concentration of the silver is known. To obtain quantitative information on AgNPs, acid dissolution of the particles was performed before TS-FF-AAS analysis, and recoveries of 80-110% were obtained.

  16. Graphite Oxidation Thermodynamics/Reactions

    Energy Technology Data Exchange (ETDEWEB)

    Propp, W.A.

    1998-09-01

    The vulnerability of graphite-matrix spent nuclear fuel to oxidation by the ambient atmosphere if the fuel canister is breached was evaluated. Thermochemical and kinetic data over the anticipated range of storage temperatures (200 to 400 C) were used to calculate the times required for a total carbon mass loss of 1 mgcm-2 from a fuel specimen. At 200 C, the time required to produce even this small loss is large, 900,000 yr. However, at 400 C the time required is only 1.9 yr. The rate of oxidation at 200 C is negligible, and the rate even at 400 C is so small as to be of no practical consequence. Therefore, oxidation of the spent nuclear fuel upon a loss of canister integrity is not anticipated to be a concern based upon the results of this study.

  17. Mass removal by oxidation and sublimation of porous graphite during fiber laser irradiation

    Science.gov (United States)

    Phillips, Grady T.; Bauer, William A.; Fox, Charles D.; Gonzales, Ashley E.; Herr, Nicholas C.; Gosse, Ryan C.; Perram, Glen P.

    2017-01-01

    The various effects of laser heating of carbon materials are key to assessing laser weapon effectiveness. Porous graphite plates, cylinders, and cones with densities of 1.55 to 1.82 g/cm3 were irradiated by a 10-kW fiber laser at 0.075 to 3.525 kW/cm2 for 120 s to study mass removal and crater formation. Surface temperatures reached steady state values as high as 3767 K. The total decrease in sample mass ranged from 0.06 to 6.29 g, with crater volumes of 0.52 to 838 mm3, and penetration times for 12.7-mm-thick plates as short as 38 s. Minor contaminants in the graphite samples produced calcium and iron oxide to be redeposited on the graphite surface. Dramatic graphite crystalline structures are also produced at higher laser irradiances. Significantly increased porosity of the sample is observed even outside the laser-irradiated region. Total mass removed increases with deposited laser energy at a rate of 4.83 g/MJ for medium extruded graphite with an apparent threshold of 0.15 MJ. At ˜3.5 kW/cm2, the fractions of the mass removed from the cylindrical samples in the crater, surrounding trench, and outer region of decreased porosity are 38%, 47%, and 15%, respectively. Graphite is particularly resistant to damage by high power lasers. The new understanding of graphite combustion and sublimation during laser irradiation is vital to the more complex behavior of carbon composites.

  18. Study of graphitic microstructure formation in diamond bulk by pulsed Bessel beam laser writing

    Science.gov (United States)

    Kumar, S.; Sotillo, B.; Chiappini, A.; Ramponi, R.; Di Trapani, P.; Eaton, S. M.; Jedrkiewicz, O.

    2017-11-01

    The advantages of using Bessel beams for the generation of graphitic structures in diamond bulk are presented. We show that by irradiating the sample with a pulsed Bessel beam whose non-diffracting zone is of the same order of the sample thickness, it is possible to produce without any sample translation straight graphitic through-microstructures, whose size depends on the input pulse energy. The microstructure growth is investigated as a function of the number of irradiating pulses, and the femtosecond and picosecond regimes are contrasted.

  19. Microextraction Methods for Preconcentration of Aluminium in Urine Samples

    Directory of Open Access Journals (Sweden)

    Farzad Farajbakhsh, Mohammad Amjadi, Jamshid Manzoori, Mohammad R. Ardalan, Abolghasem Jouyban

    2016-07-01

    Full Text Available Background: Analysis of aluminium (Al in urine samples is required in management of a number of diseases including patients with renal failure. This work aimed to present dispersive liquid-liquid microextraction (DLLME and ultrasound-assisted emulsification microextraction (USAEME methods for the preconcentration of ultra-trace amount of aluminum in human urine prior to its determination by a graphite furnace atomic absorption spectrometry (GFAAS. Methods: The microextraction methods were based on the complex formation of Al3+ with 8-hydroxyquinoline. The effect of various experimental parameters on the efficiencies of the methods and their optimum values were studied. Results: Under the optimal conditions, the limits of detection for USAEME-GFAAS and DLLME-GFAAS were 0.19 and 0.30 ng mL−1, respectively and corresponding relative standard deviations (RSD, n=5 for the determination of 40 ng mL−1 Al3+ were 5.9% and 4.9%. Conclusion: Both methods could be successfully used to the analysis of ultra trace concentrations of Al in urine samples of dialysis patients.

  20. Method for molding threads in graphite panels

    Science.gov (United States)

    Short, W.W.; Spencer, C.

    1994-11-29

    A graphite panel with a hole having a damaged thread is repaired by drilling the hole to remove all of the thread and making a new hole of larger diameter. A bolt with a lubricated thread is placed in the new hole and the hole is packed with graphite cement to fill the hole and the thread on the bolt. The graphite cement is cured, and the bolt is unscrewed therefrom to leave a thread in the cement which is at least as strong as that of the original thread. 8 figures.

  1. Status of Chronic Oxidation Studies of Graphite

    Energy Technology Data Exchange (ETDEWEB)

    Contescu, Cristian I. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Mee, Robert W. [Univ. of Tennessee, Knoxville, TN (United States)

    2016-05-01

    Graphite will undergo extremely slow, but continuous oxidation by traces of moisture that will be present, albeit at very low levels, in the helium coolant of HTGR. This chronic oxidation may cause degradation of mechanical strength and thermal properties of graphite components if a porous oxidation layer penetrates deep enough in the bulk of graphite components during the lifetime of the reactor. The current research on graphite chronic oxidation is motivated by the acute need to understand the behavior of each graphite grade during prolonged exposure to high temperature chemical attack by moisture. The goal is to provide the elements needed to develop predictive models for long-time oxidation behavior of graphite components in the cooling helium of HTGR. The tasks derived from this goal are: (1) Oxidation rate measurements in order to determine and validate a comprehensive kinetic model suitable for prediction of intrinsic oxidation rates as a function of temperature and oxidant gas composition; (2) Characterization of effective diffusivity of water vapor in the graphite pore system in order to account for the in-pore transport of moisture; and (3) Development and validation of a predictive model for the penetration depth of the oxidized layer, in order to assess the risk of oxidation caused damage of particular graphite grades after prolonged exposure to the environment of helium coolant in HTGR. The most important and most time consuming of these tasks is the measurement of oxidation rates in accelerated oxidation tests (but still under kinetic control) and the development of a reliable kinetic model. This report summarizes the status of chronic oxidation studies on graphite, and then focuses on model development activities, progress of kinetic measurements, validation of results, and improvement of the kinetic models. Analysis of current and past results obtained with three grades of showed that the classical Langmuir-Hinshelwood model cannot reproduce all

  2. Adsorption of lead over graphite oxide.

    Science.gov (United States)

    Olanipekun, Opeyemi; Oyefusi, Adebola; Neelgund, Gururaj M; Oki, Aderemi

    2014-01-24

    The adsorption efficiency and kinetics of removal of lead in presence of graphite oxide (GO) was determined using the Atomic Absorption Spectrophotometer (AAS). The GO was prepared by the chemical oxidation of graphite and characterized using FTIR, SEM, TGA and XRD. The adsorption efficiency of GO for the solution containing 50, 100 and 150 ppm of Pb(2+) was found to be 98%, 91% and 71% respectively. The adsorption ability of GO was found to be higher than graphite. Therefore, the oxidation of activated carbon in removal of heavy metals may be a viable option to reduce pollution in portable water. Published by Elsevier B.V.

  3. Synthesis of soluble graphite and graphene.

    Science.gov (United States)

    Kelly, K F; Billups, W E

    2013-01-15

    Because of graphene's anticipated applications in electronics and its thermal, mechanical, and optical properties, many scientists and engineers are interested in this material. Graphene is an isolated layer of the π-stacked hexagonal allotrope of carbon known as graphite. The interlayer cohesive energy of graphite, or exfoliation energy, that results from van der Waals attractions over the interlayer spacing distance of 3.34 Å (61 meV/C atom) is many times weaker than the intralayer covalent bonding. Since graphene itself does not occur naturally, scientists and engineers are still learning how to isolate and manipulate individual layers of graphene. Some researchers have relied on the physical separation of the sheets, a process that can sometimes be as simple as peeling of sheets from crystalline graphite using Scotch tape. Other researchers have taken an ensemble approach, where they exploit the chemical conversion of graphite to the individual layers. The typical intermediary state is graphite oxide, which is often produced using strong oxidants under acidic conditions. Structurally, researchers hypothesize that acidic functional groups functionalize the oxidized material at the edges and a network of epoxy groups cover the sp(2)-bonded carbon network. The exfoliated material formed under these conditions can be used to form dispersions that are usually unstable. However, more importantly, irreversible defects form in the basal plane during oxidation and remain even after reduction of graphite oxide back to graphene-like material. As part of our interest in the dissolution of carbon nanomaterials, we have explored the derivatization of graphite following the same procedures that preserve the sp(2) bonding and the associated unique physical and electronic properties in the chemical processing of single-walled carbon nanotubes. In this Account, we describe efficient routes to exfoliate graphite either into graphitic nanoparticles or into graphene without

  4. Qualitative and quantitative analysis of N-acetyllactosamine and lacto-N-biose, the two major building blocks of human milk oligosaccharides in human milk samples by high-performance liquid chromatography-tandem mass spectrometry using a porous graphitic carbon column.

    Science.gov (United States)

    Balogh, Réka; Jankovics, Péter; Béni, Szabolcs

    2015-11-27

    This study presents a validated, porous graphitic carbon stationary phase-based LC-MS/MS method for the identification and quantification of lacto-N-biose (LNB) and N-acetyllactosamine (LacNAc). These compounds are the major building blocks of human milk oligosaccharides, however the presence of their unbound form in human milk has not been examined so far. The separation of these highly related structures in their alditol form was accomplished by a gradient LC method and multiple reaction monitoring (MRM) analysis after appropriate sample preparation including size-exclusion chromatography and solid-phase extraction. Baseline separation of the components provides the selectivity for the method. Validation was performed according to the European Medicines Agency (EMA) Guidelines and the method was found to be precise and accurate. Using our developed and validated method we were able to identify and quantify both saccharides in human milk for the first time. Based on our results the LacNAc concentration is in the range of 6.7-31μg/mL while LNB concentration decreased from 26μg/mL below the detection limit during the first week of lactation. The presence of LNB and LacNAc in human milk also implies new biological functions which can lead us closer to the understanding of the various functions of this complex biofluid. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Synthesis of graphitic carbon nitride by reaction of melamine and uric acid

    Energy Technology Data Exchange (ETDEWEB)

    Dante, Roberto C., E-mail: rcdante@yahoo.com [Laboratorio de Tecnologias del Medio Ambiente, Departamento de Ingenieria Agricola y Forestal, Universidad de Valladolid, Avenida de Madrid 44, 34004 Palencia (Spain); Martin-Ramos, Pablo, E-mail: pablomartinramos@gmail.com [Laboratorio de Tecnologias del Medio Ambiente, Departamento de Ingenieria Agricola y Forestal, Universidad de Valladolid, Avenida de Madrid 44, 34004 Palencia (Spain); Correa-Guimaraes, Adriana, E-mail: acg@iaf.uva.es [Laboratorio de Tecnologias del Medio Ambiente, Departamento de Ingenieria Agricola y Forestal, Universidad de Valladolid, Avenida de Madrid 44, 34004 Palencia (Spain); Martin-Gil, Jesus, E-mail: jesusmartingil@gmail.com [Laboratorio de Tecnologias del Medio Ambiente, Departamento de Ingenieria Agricola y Forestal, Universidad de Valladolid, Avenida de Madrid 44, 34004 Palencia (Spain)

    2011-11-01

    Highlights: {yields} Graphitic carbon nitrides by CVD of melamine and uric acid on alumina. {yields} The building blocks of carbon nitrides are heptazine nuclei. {yields} Composite particles with alumina core and carbon nitride coating. - Abstract: Graphitic carbon nitrides were synthesized starting from melamine and uric acid. Uric acid was chosen because it thermally decomposes, and reacts with melamine by condensation at temperatures in the range of 400-600 deg. C. The reagents were mixed with alumina and subsequently the samples were treated in an oven under nitrogen flux. Alumina favored the deposition of the graphitic carbon nitrides layers on the exposed surface. This method can be assimilated to an in situ chemical vapor deposition (CVD). Infrared (IR) spectra, as well as X-ray diffraction (XRD) patterns, are in accordance with the formation of a graphitic carbon nitride with a structure based on heptazine blocks. These carbon nitrides exhibit poor crystallinity and a nanometric texture, as shown by transmission electron microscopy (TEM) analysis. The thermal degradation of the graphitic carbon nitride occurs through cyano group formation, and involves the bridging tertiary nitrogen and the bonded carbon, which belongs to the heptazine ring, causing the ring opening and the consequent network destruction as inferred by connecting the IR and X-ray photoelectron spectroscopy (XPS) results. This seems to be an easy and promising route to synthesize graphitic carbon nitrides. Our final material is a composite made of an alumina core covered by carbon nitride layers.

  6. Nanostructured composite material graphite/TiO2 and its antibacterial activity under visible light irradiation.

    Science.gov (United States)

    Dědková, Kateřina; Lang, Jaroslav; Matějová, Kateřina; Peikertová, Pavlína; Holešinský, Jan; Vodárek, Vlastimil; Kukutschová, Jana

    2015-08-01

    The paper addresses laboratory preparation, characterization and in vitro evaluation of antibacterial activity of graphite/TiO2 nanocomposites. Composites graphite/TiO2 with various ratio of TiO2 nanoparticles (30wt.%, and 50wt.%) to graphite were prepared using a thermal hydrolysis of titanylsulfate in the presence of graphite particles, and subsequently dried at 80°C. X-ray powder diffraction, transmission electron microscopy and Raman microspectroscopy served as phase-analytical methods distinguishing anatase and rutile phases in the prepared composites. Scanning and transmission electron microscopy techniques were used for characterization of morphology of the prepared samples. A developed modification of the standard microdilution test was used for in vitro evaluation of daylight induced antibacterial activity, using four common human pathogenic bacterial strains (Staphylococcus aureus, Escherichia coli, Enterococcus faecalis and Pseudomonas aeruginosa). Antibacterial activity of the graphite/TiO2 nanocomposites could be based mainly on photocatalytic reaction with subsequent potential interaction of reactive oxygen species with bacterial cells. During the antibacterial activity experiments, the graphite/TiO2 nanocomposites exhibited antibacterial activity, where differences in the onset of activity and activity against bacterial strains were observed. The highest antibacterial activity evaluated as minimum inhibitory concentration was observed against P. aeruginosa after 180min of irradiation. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Comparison on graphite, graphene oxide and reduced graphene oxide: Synthesis and characterization

    Science.gov (United States)

    Hidayah, N. M. S.; Liu, Wei-Wen; Lai, Chin-Wei; Noriman, N. Z.; Khe, Cheng-Seong; Hashim, U.; Lee, H. Cheun

    2017-10-01

    Graphene oxide (GO) and reduced graphene oxide (RGO) are known to have superior properties for various applications. This work compares the properties of GO and RGO with graphite. GO was prepared by using Improved Hummer's method whereas the produced GO was subjected to chemical reduction with the use of hydrazine hydrate. Graphite, GO and RGO had different morphologies, quality, functionalized groups, UV-Vis absorption peaks and crystallinity. With the removal of oxygen-containing functional group during reduction for RGO, the quality of samples was decreased due to higher intensity of D band than G band was seen in Raman results. In addition, platelet-like surface can be observed on the surface of graphite as compared to GO and RGO where wrinkled and layered flakes, and crumpled thin sheets were observed on GO and RGO surface respectively. Fourier Transform Infra-Red (FTIR) analysis showed the presence of abundant oxygen-containing functional groups in GO as compared to RGO and graphite. The characteristic peaks at 26.62°, 9.03° and 24.10° for graphite, GO and RGO, respectively, can be detected from X-Ray diffraction (XRD). Furthermore, the reduction also caused red shift at 279nm from 238nm, as obtained from ultraviolet visible (UV-Vis) analysis. The results proved that GO was successfully oxidized from graphite whereas RGO was effectively reduced from GO.

  8. LEO degradation of graphite and carbon-based composites aboard Space Shuttle Flight STS-46

    Science.gov (United States)

    Spady, Blaine R.; Synowicki, R. A.; Hale, Jeffrey S.; Devries, M. J.; Woollam, John A.; Moore, Arthur W.; Lake, Max

    1995-01-01

    Six different types of carbon and carbon-boron nitride composites were exposed to low Earth orbit aboard Space Shuttle flight STS-46. The samples received a nominal atomic oxygen fluence of 2.2 x 10(exp 20) atoms/sq cm in 42 hours of exposure. Pyrolytic graphite and highly oriented pyrolytic graphite showed significant degradation, and the measured erosion yield was within a factor of two of published values. The erosion yield of pyrolytic boron nitride was found to be 2.6 x 10(exp 26) cu cm/atom in plasma asher exposure, over 42 times lower than that of pyrolytic graphite. This low erosion yield makes graphite plus boron nitride mixtures quite resistant to low Earth orbit exposure. Evidence suggests that the graphitic component was preferentially etched, leaving the surface boron nitride rich. Degradation resistance increases with boron nitride composition. Carbon fiber/carbon composites degraded in low Earth orbit, and the carbon pitch binder was found to etch more easily than the graphite fibers which have much higher degradation resistance.

  9. Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nischkauer, Winfried [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); Herincs, Esther [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Puschenreiter, Markus; Wenzel, Walter [University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Limbeck, Andreas, E-mail: A.Limbeck@tuwien.ac.at [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria)

    2013-11-01

    Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g{sup −1}, 0.14 μg g{sup −1} and 0.13 μg g{sup −1} were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was

  10. Performance of AC/graphite capacitors at high weight ratios of AC/graphite

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Hongyu [IM and T Ltd., Advanced Research Center, Saga University, 1341 Yoga-machi, Saga 840-0047 (Japan); Yoshio, Masaki [Advanced Research Center, Department of Applied Chemistry, Saga University, 1341 Yoga-machi, Saga 840-0047 (Japan)

    2008-03-01

    The effect of negative to positive electrode materials' weight ratio on the electrochemical performance of both activated carbon (AC)/AC and AC/graphite capacitors has been investigated, especially in the terms of capacity and cycle-ability. The limited capacity charge mode has been proposed to improve the cycle performance of AC/graphite capacitors at high weight ratios of AC/graphite. (author)

  11. Evaluation of the graphite electrode arc melter for processing heterogeneous waste

    Energy Technology Data Exchange (ETDEWEB)

    O' Connor, William K.; Turner, Paul C.; Soelberg, N.R. (Idaho National Engineering Laboratory); Anderson, G.L. (Idaho National Engineering Laboratory)

    1996-01-01

    The U.S. Bureau of Mines (USBM) conducted a series of 4 demonstration melting tests in a 3-phase AC graphite electrode arc furnace at its Albany Research Center (ALRC) thermal treatment facility in Albany, Oregon (now part of the U.S. Department of Energy, DOE). The scope of these tests provides a unique opportunity to evaluate a single melting technology regarding its applicability to the treatment of several different heterogeneous mixed wastes. The current system can continuously process combustible-bearing wastes at feedrates to 682 kg/h (1,500 lb/h), continuously tap slag or glass, and intermittently tap metal products, and includes a close-coupled thermal oxidizer and air pollution control system (APCS). The 4 demonstration melting tests were conducted in cooperation with the American Society of Mechanical Engineers (ASME), the Idaho National Engineering Laboratory (INEL), and the Westinghouse Hanford Company (WHC).

  12. Nano-scale orientation mapping of graphite in cast irons

    Energy Technology Data Exchange (ETDEWEB)

    Theuwissen, Koenraad; Lacaze, Jacques [Institut CARNOT CIRIMAT, Université de Toulouse, ENSIACET, CS 44362, 31030 Toulouse Cedex 4 (France); Véron, Muriel [SIMAP, CNRS-Grenoble INP, BP 46 101 rue de la Physique, 38402 Saint Martin d' Hères (France); Laffont, Lydia, E-mail: lydia.laffont@ensiacet.fr [Institut CARNOT CIRIMAT, Université de Toulouse, ENSIACET, CS 44362, 31030 Toulouse Cedex 4 (France)

    2014-09-15

    A diametrical section of a graphite spheroid from a ductile iron sample was prepared using the focused ion beam-lift out technique. Characterization of this section was carried out through automated crystal orientation mapping in a transmission electron microscope. This new technique automatically collects electron diffraction patterns and matches them with precalculated templates. The results of this investigation are crystal orientation and phase maps of the specimen, which bring new light to the understanding of growth mechanisms of this peculiar graphite morphology. This article shows that mapping the orientation of carbon-based materials such as graphite, which is difficult to achieve with conventional techniques, can be performed automatically and at high spatial resolution using automated crystal orientation mapping in a transmission electron microscope. - Highlights: • ACOM/TEM can be used to study the crystal orientation of carbon-based materials. • A spheroid is formed by conical sectors radiating from a central nuclei. • Misorientations exist within the conical sectors, defining various orientation domains.

  13. Carbon Nanotubes Growth by CVD on Graphite Fibers

    Science.gov (United States)

    Zhu, Shen; Su, Ching-Hua; Cochrane, J. C.; Lehoczky, S. L.; Muntele, I.; Ila, D.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    Due to the superior electrical and mechanical properties of carbon nanotubes (CNT), synthesizing CNT on various substances for electronics devices and reinforced composites have been engaged in many efforts for applications. This presentation will illustrate CNT synthesized on graphite fibers by thermal CVD. On the fiber surface, iron nanoparticles as catalysts for CNT growth are coated. The growth temperature ranges from 600 to 1000 C and the pressure ranges from 100 Torr to one atmosphere. Methane and hydrogen gases with methane content of 10% to 100% are used for the CNT synthesis. At high growth temperatures (greater than or equal to 900 C), the rapid inter-diffusion of the transition metal iron on the graphite surface results in the rough fiber surface without any CNT grown on it. When the growth temperature is relative low (650-800 C), CNT with catalytic particles on the nanotube top ends are fabricated on the graphite surface. (Methane and hydrogen gases with methane content of 10% to 100% are used for the CNT synthesis.) (By measuring the samples) Using micro Raman spectroscopy in the breath mode region, single-walled or multi-walled CNT (MWCNT), depending on growth concentrations, are found. Morphology, length and diameter of these MWCNT are determined by scanning electron microscopy and Raman spectroscopy. The detailed results of syntheses and characterizations will be discussed in the presentation.

  14. Mechanical Degradation of Graphite/PVDF Composite Electrodes: A Model-Experimental Study

    Energy Technology Data Exchange (ETDEWEB)

    Takahashi, K; Higa, K; Mair, S; Chintapalli, M; Balsara, N; Srinivasan, V

    2015-12-11

    Mechanical failure modes of a graphite/polyvinylidene difluoride (PVDF) composite electrode for lithium-ion batteries were investigated by combining realistic stress-stain tests and mathematical model predictions. Samples of PVDF mixed with conductive additive were prepared in a similar way to graphite electrodes and tested while submerged in electrolyte solution. Young's modulus and tensile strength values of wet samples were found to be approximately one-fifth and one-half of those measured for dry samples. Simulations of graphite particles surrounded by binder layers given the measured material property values suggest that the particles are unlikely to experience mechanical damage during cycling, but that the fate of the surrounding composite of PVDF and conductive additive depends completely upon the conditions under which its mechanical properties were obtained. Simulations using realistic property values produced results that were consistent with earlier experimental observations.

  15. Comparative study of porosity and pores morphology of unalloyed iron sintered in furnace and plasma reactor

    Directory of Open Access Journals (Sweden)

    Henrique Cezar Pavanati

    2007-03-01

    Full Text Available Samples of unalloyed iron were sintered in the presence of an abnormal glow discharge using a confined anode-cathode configuration. The samples were placed on a holder acting as the discharge anode inside an AISI 1020 steel hollow cathode. Heating of the outer cathode was obtained by the bombardment of ions and energetic neutral particles. As a consequence of the confined geometry, the sample was efficiently heated mainly by radiation from the cathode. In order to evaluate the results of the sintering process by plasma, samples of unalloyed iron were also sintered in a resistive furnace using the same thermal cycle. The porosity, dimension and morphology of the pores were characterized by means of four basic parameters: area fraction, mean diameter, shape factor and elongation factor. The results show that the shape factor depends on the pore size, a characteristic that was not observed for elongation factor. For samples sintered in plasma reactor or conventional furnace, no significant difference in the porosity or in the pores morphology was observed.

  16. Multi-impregnating pitch-bonded Egyptian dolomite refractory brick for application in ladle furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Rabah, M.; Ewais, E.M.M. [CMRDI, Cairo (Egypt)

    2009-03-15

    A method of preparation of multi-impregnated pitch-bonded Egyptian dolomite refractory brick for ladle furnace is described. Brick samples were prepared from blend of calcined dolomite mineral and coal tar pitch. The blend was hot mixed and pressed under a compression force up to 151 MPa. Green bricks were baked for 2 h at temperatures up to 1000 {sup o}C. Voids in the baked bodies were filled with carbon by multiple impregnations using low-softening point coal tar pitch. Each impregnation step (30 min) was followed by calcination at 1000 degrees C. Brick samples containing 8-12 wt.% coal tar pitch binder and pressed under 108-151 MPa acquired quantify crushing strength. However, multi-impregnating favored the mechanical strength of the baked brick samples and improved their hydration resistance (>45 days). Dolomite brick samples containing 10 wt.% coal tar pitch and pressed at 108 MPa gave high hydration resistance (more than 60 days in normal condition) compared to the hydration resistance of the commercial bricks (30 days). The prepared brick samples have acceptable density, chemical stability, outstanding resistance and good mechanical properties would meet the requirements of Ladle furnace (LF) for steel making industry. In addition, estimation of production cost of the brick indicates it is competitive with the market price based on durability and service life time aspects.

  17. Model reduction for experimental thermal characterization of a holding furnace

    Science.gov (United States)

    Loussouarn, Thomas; Maillet, Denis; Remy, Benjamin; Dan, Diane

    2017-09-01

    Vacuum holding induction furnaces are used for the manufacturing of turbine blades by loss wax foundry process. The control of solidification parameters is a key factor for the manufacturing of these parts. The definition of the structure of a reduced heat transfer model with experimental identification through an estimation of its parameters is required here. Internal sensors outputs, together with this model, can be used for assessing the thermal state of the furnace through an inverse approach, for a better control. Here, an axisymmetric furnace and its load have been numerically modelled using FlexPDE, a finite elements code. The internal induction heat source as well as the transient radiative transfer inside the furnace are calculated through this detailed model. A reduced lumped body model has been constructed to represent the numerical furnace. The model reduction and the estimation of the parameters of the lumped body have been made using a Levenberg-Marquardt least squares minimization algorithm, using two synthetic temperature signals with a further validation test.

  18. Fabrication of Iron-Containing Carbon Materials From Graphite Fluoride

    Science.gov (United States)

    Hung, Ching-cheh

    1996-01-01

    Carbon materials containing iron alloy, iron metal, iron oxide or iron halide were fabricated. Typical samples of these metals were estimated to contain 1 iron atom per 3.5 to 5 carbon atoms. Those carbon materials containing iron alloy, iron metal, and/or Fe3O4 were magnetic. The kinetics of the fabrication process were studied by exposing graphite fluoride (CF(0.68)) to FeCl3 over a 280 to 420 C temperature range. Between 280 and 295 C, FeCl3 quickly entered the structure of CF(0.68), broke the carbon-fluorine bonds, and within 10 to 30 min, completely converted it to carbon made up of graphite planes between which particles of crystalline FeF3 and noncrystalline FeCl3 were located. Longer reaction times (e.g., 28 hr) or higher reaction temperatures (e.g., 420 C) produced materials containing graphite, a FeCl3-graphite intercalation compound, FeCl2(center dot)4H2O, and FeCl2(center dot)2H2O. These products were further heat treated to produce iron-containing carbon materials. When the heating temperature was kept in the 750 to 850 C range, and the oxygen supply was kept at the optimum level, the iron halides in the carbon structure were converted to iron oxides. Raising the heat to temperatures higher than 900 C reduced such iron oxides to iron metal. The kinetics of these reactions were used to suggest processes for fabricating carbon materials containing iron alloy. Such processes were then tested experimentally. In one of the successful trial runs, commercially purchased CF(0.7) powder was used as the reactant, and NiO was added during the final heating to 1200 C as a source of both nickel and oxygen. The product thus obtained was magnetic and was confirmed to be a nickel-iron alloy in carbon.

  19. Ballistic Diffusion in Polyaromatic Hydrocarbons on Graphite.

    Science.gov (United States)

    Calvo-Almazán, Irene; Sacchi, Marco; Tamtögl, Anton; Bahn, Emanuel; Koza, Marek M; Miret-Artés, Salvador; Fouquet, Peter

    2016-12-15

    This work presents an experimental picture of molecular ballistic diffusion on a surface, a process that is difficult to pinpoint because it generally occurs on very short length scales. By combining neutron time-of-flight data with molecular dynamics simulations and density functional theory calculations, we provide a complete description of the ballistic translations and rotations of a polyaromatic hydrocarbon (PAH) adsorbed on the basal plane of graphite. Pyrene, C16H10, adsorbed on graphite is a unique system, where at relative surface coverages of about 10-20% its mean free path matches the experimentally accessible time/space scale of neutron time-of-flight spectroscopy (IN6 at the Institut Laue-Langevin). The comparison between the diffusive behavior of large and small PAHs such as pyrene and benzene adsorbed on graphite brings a strong experimental indication that the interaction between molecules is the dominating mechanism in the surface diffusion of polyaromatic hydrocarbons adsorbed on graphite.

  20. Graphite: An active or an inactive anode?

    Energy Technology Data Exchange (ETDEWEB)

    Rueffer, Matthew; Bejan, Dorin [Electrochemical Technology Centre, Chemistry Department, University of Guelph, 50 Stone Road East, Guelph Ontario, N1G 2W1 (Canada); Bunce, Nigel J., E-mail: nbunce@uoguelph.c [Electrochemical Technology Centre, Chemistry Department, University of Guelph, 50 Stone Road East, Guelph Ontario, N1G 2W1 (Canada)

    2011-02-01

    Positive polarization of a graphite anode in aqueous solution functionalizes the surface and releases soluble organic carbon to the solution concurrent with the electrolysis of water. Mineralization of the anode occurs at more positive potentials, and can be explained as a repetitive sequence involving functionalization, oxidation to carboxyl, and Kolbe decarboxylation, without recourse to hydroxyl radicals. Other lines of evidence against the intermediacy of hydroxyl radicals include the resistance of p-benzoquinone towards oxidation at graphite - i.e., graphite does not function as an inactive anode towards the oxidation of added substrates. A direct electron transfer mechanism operates for substrates that are oxidizable in the range of water stability, such as acetaminophen and sulfide ion. In the potential range of oxygen evolution we propose that graphite behaves as a modified active anode, at which the oxygen atom to be transferred to an oxidizable substrate first becomes bonded to the previously functionalized surface.

  1. Graphite Oxide and Aromatic Amines : Size Matters

    NARCIS (Netherlands)

    Spyrou, Konstantinos; Calvaresi, Matteo; Diamanti, Evmorfi A. K.; Tsoufis, Theodoros; Gournis, Dimitrios; Rudolf, Petra; Zerbetto, Francesco

    2015-01-01

    Experimental and theoretical studies are performed in order to illuminate, for first time, the intercalation mechanism of polycyclic aromatic molecules into graphite oxide. Two representative molecules of this family, aniline and naphthalene amine are investigated. After intercalation, aniline

  2. Hydrogen storage properties on mechanically milled graphite

    OpenAIRE

    Ichikawa, Takayuki; Chen, D. M.; Isobe, Shigehito; Gomibuchi, Emi; Fujii, Hironobu

    2004-01-01

    We investigated hydrogen absorption/desorption and structural properties in mechanically milled graphite under hydrogen pressures up to 6 MPa to clarify catalytic and hydrogen pressure effects in the milling. The results indicate that a small amount of iron contamination during milling plays a quite important role as a catalyst for hydrogen absorption/desorption properties in graphite. Two-peak structure for hydrogen desorption in the TDS profile is due to existence of two different occupatio...

  3. Graphite Composite Panel Polishing Fixture

    Science.gov (United States)

    Hagopian, John; Strojny, Carl; Budinoff, Jason

    2011-01-01

    The use of high-strength, lightweight composites for the fixture is the novel feature of this innovation. The main advantage is the light weight and high stiffness-to-mass ratio relative to aluminum. Meter-class optics require support during the grinding/polishing process with large tools. The use of aluminum as a polishing fixture is standard, with pitch providing a compliant layer to allow support without deformation. Unfortunately, with meter-scale optics, a meter-scale fixture weighs over 120 lb (.55 kg) and may distort the optics being fabricated by loading the mirror and/or tool used in fabrication. The use of composite structures that are lightweight yet stiff allows standard techniques to be used while providing for a decrease in fixture weight by almost 70 percent. Mounts classically used to support large mirrors during fabrication are especially heavy and difficult to handle. The mount must be especially stiff to avoid deformation during the optical fabrication process, where a very large and heavy lap often can distort the mount and optic being fabricated. If the optic is placed on top of the lapping tool, the weight of the optic and the fixture can distort the lap. Fixtures to support the mirror during fabrication are often very large plates of aluminum, often 2 in. (.5 cm) or more in thickness and weight upwards of 150 lb (68 kg). With the addition of a backing material such as pitch and the mirror itself, the assembly can often weigh over 250 lb (.113 kg) for a meter-class optic. This innovation is the use of a lightweight graphite panel with an aluminum honeycomb core for use as the polishing fixture. These materials have been used in the aerospace industry as structural members due to their light weight and high stiffness. The grinding polishing fixture consists of the graphite composite panel, fittings, and fixtures to allow interface to the polishing machine, and introduction of pitch buttons to support the optic under fabrication. In its

  4. Radiation cured epoxy acrylate composites based on graphene, graphite oxide and functionalized graphite oxide with enhanced properties.

    Science.gov (United States)

    Guo, Yuqiang; Bao, Chenlu; Song, Lei; Qian, Xiaodong; Yuan, Bihe; Hu, Yuan

    2012-03-01

    Epoxy acrylate (EA) composites containing graphite oxide (GO), graphene and nitrogen-double bond functionalized graphite oxide (FGO) were fabricated using UV-radiation and electron beam radiation via in-situ polymerization. Graphene and FGO were homogenously dispersed in EA matrix and enhanced properties, including thermal stability, flame retardancy, electrical conductivity and reduced deleterious gas releasing in thermo decomposition were obtained. Microscale combustion colorimeter results illustrated improved flame retardancy; EA/FGO composites achieved a 29.7% reduction in total heat release (THR) when containing only 0.1% FGO and a 38.6% reduction in peak-heat release rate (PHRR) when containing 3% FGO. The onset decomposition temperatures were delayed and the maximum decomposition values were reduced, according to thermogravimetric analysis which indicated enhanced thermal stabilities. The electrical conductivity was increased by 6 orders of magnitude (3% graphene) and the deleterious gas released during the thermo decomposition was reduced with the addition of all the graphite samples. This study represented a new approach to functionalize GO with flame retardant elements and active curable double bond to achieve better dispersion of GO into polymer matrix to obtain nanocomposites and paved a way for achieving graphene-based materials with high-performance of graphene in enhancement of flame retardancy of polymers for practical applications.

  5. Structure and functionality of bromine doped graphite.

    Science.gov (United States)

    Hamdan, Rashid; Kemper, A F; Cao, Chao; Cheng, H P

    2013-04-28

    First-principles calculations are used to study the enhanced in-plane conductivity observed experimentally in Br-doped graphite, and to study the effect of external stress on the structure and functionality of such systems. The model used in the numerical calculations is that of stage two doped graphite. The band structure near the Fermi surface of the doped systems with different bromine concentrations is compared to that of pure graphite, and the charge transfer between carbon and bromine atoms is analyzed to understand the conductivity change along different high symmetry directions. Our calculations show that, for large interlayer separation between doped graphite layers, bromine is stable in the molecular form (Br2). However, with increased compression (decreased layer-layer separation) Br2 molecules tend to dissociate. While in both forms, bromine is an electron acceptor. The charge exchange between the graphite layers and Br atoms is higher than that with Br2 molecules. Electron transfer to the Br atoms increases the number of hole carriers in the graphite sheets, resulting in an increase of conductivity.

  6. Intumescent mechanisms of fire-retarding polyurethane systems and development of graphite/polymer nano-composites

    Science.gov (United States)

    Yuan, Qingchun

    As an effective and environmentally friendly fire retarding approach, intumescence has been applied to design better fire retarding polymer systems for different applications. However, intumescent mechanisms have not been well understood. This has hindered the further development of intumescent fire retarding polymer systems. This research investigated the intumescent mechanisms of three commercial fire retarding polyurethane products and developed a new generation of fire retarding products based on graphite/polymer nanocomposites. The three commercial products were studied using a single direction well-ventilated natural burning method and a series of intumescent char characterisation techniques developed in this research. The natural burning method was designed to show the protection and protection efficiency of intumescent chars. The protection efficiency was measured by the difference of char yields between natural burning and furnace burning. The intumescent chars produced by natural burning were investigated for their char structures, gas permeability, bulk strength and reactivity using microscopic methods, open porosity, durometer hardness and X-ray diffraction, respectively. Experimental results show that the three commercial products contain inert inorganic additives. The charring ability of the polymers is important in producing integrated chars by binding the inert additives together, and in strengthening the chars. An integrated char with lower open porosity has higher protection efficiency. The lower porosity also results in the char with higher strength. Graphite/polymer nanocomposites were synthesised by solution intercalation and in situ polymerisation methods. Five graphites were modified into graphite oxides (GO) by oxidation. A chosen GO was intercalated with a polyethylene oxide (PEO), polyethylene glycol Mn300 (PEG1500) or polyvinyl pyrrolidone (PVP) in water. The GO and its PEG1500 or PVP intercalated compounds as nano-structured graphites

  7. Compacting of fly dusts from cupola and electric arc furnace

    Directory of Open Access Journals (Sweden)

    D. Baricová

    2012-01-01

    Full Text Available Recycling and utilization of dust waste is important not only from the point of view of its usage as an alternative source of raw materials, but regarding the environmental problems also. Dust emissions arise from thermal and chemical or physical processes and mechanical actions. Two kinds of fl y dusts from cupola furnaces (hot and cold blast cupola furnace and fl y dust from electric arc furnace were used by experiments. They were pelletized only with addition of water and briquetted with diff erent addition of water glass, bentonite and cement. Quality of briquettes was tested by compression – strength test and by break down test in green state, after drying and afterstoring (1 month.

  8. Gas dynamics of reactive gases in swirling-type furnace

    Science.gov (United States)

    Akhmetshina, A. I.; Pavlov, G. I.; Sabirzyanov, A. N.; Tikhonov, O. A.

    2017-09-01

    It is known from the literature that for the complete reaction of two gases (fuel and oxidizer), it is necessary to fulfill three basic conditions: the stoichiometric ratio of reactive gases, qualitative mixing and ensuring the cooling of combustion products without "quenching". Of the above-stated conditions it is more difficult to organize a qualitative mixture formation. This physical process requires additional expenditure of energy flow. In this work we present the results of experimental and theoretical studies of the gas dynamics of a reactive gas mixture in a swirling-type furnace. The design scheme of the furnace includes two reaction zones for combustible components: the first zone is the zone of generation of combustible gases which composition is constant; the second zone of the furnace - zone of a homogeneous combustion reaction.

  9. A feasibility assessment of cogeneration from a regenerative glass furnace

    Energy Technology Data Exchange (ETDEWEB)

    Hnat, J.G.; Coles, W.F.

    1985-07-01

    In typical oil/gas-fired regenerative glass furnaces, approximately one-third of the total thermal input is exhausted out the stack at temperatures in the range of 700-1000/sup 0/F. The results of a site specific feasibility assessment of cogeneration from the stack gas waste heat of a regenerative glass furnace is summarized. Three different cogeneration concepts were evaluated for heat recovery. They included: a) a conventional steam Rankine cycle, b) an organic Rankine cycle, and c) a pressurized Brayton cycle. The performance and economics of the three cogeneration heat recovery systems are compared for a range of flue gas temperatures and flow rates which encompass expected operating conditions for a nominal furnace campaign period.

  10. Bulk retention of deuterium in graphites exposed to deuterium plasma at high temperature

    Energy Technology Data Exchange (ETDEWEB)

    Arkhipov, I.I. [Rossijskaya Akademiya Nauk, Moscow (Russian Federation). Inst. Fizicheskoj Khimii; Gorodetsky, A.E. [Rossijskaya Akademiya Nauk, Moscow (Russian Federation). Inst. Fizicheskoj Khimii; Zakharov, A.P. [Rossijskaya Akademiya Nauk, Moscow (Russian Federation). Inst. Fizicheskoj Khimii; Khripunov, B.I. [Institute of Nuclear Fusion, RRC `Kurchatov Institute`, Kurchatov sq. 1, 123182 Moscow (Russian Federation); Shapkin, V.V. [Institute of Nuclear Fusion, RRC `Kurchatov Institute`, Kurchatov sq. 1, 123182 Moscow (Russian Federation); Petrov, V.B. [Institute of Nuclear Fusion, RRC `Kurchatov Institute`, Kurchatov sq. 1, 123182 Moscow (Russian Federation); Pistunovich, V.I. [Institute of Nuclear Fusion, RRC `Kurchatov Institute`, Kurchatov sq. 1, 123182 Moscow (Russian Federation); Negodaev, M.A. [P.N. Lebedev Physical Institute, Russian Academy of Sciences, Leninsky pr. 53, 117924 Moscow (Russian Federation); Bagulya, A.V. [P.N. Lebedev Physical Institute, Russian Academy of Sciences, Leninsky pr. 53, 117924 Moscow (Russian Federation)

    1996-10-01

    A highly ionized deuterium plasma with a low residual gas pressure and a high intensity D{sub 2}{sup +}-ion beam were used for the study of deuterium retention in RG-Ti-91 and POCO AXF-5Q graphites. Deuterium retention in the samples was estimated by TDS during heating to 2000 K. Mechanical removal of a surface layer 100 {mu}m thick was used to distinguish bulk and surface fractions of retained deuterium. The samples of RG-Ti and POCO graphites were exposed to a plasma with an ion flux of 3 x 10{sup 17} D/cm{sup 2}.s in the `Lenta` plasma device for 10 to 10{sup 4} s at residual deuterium pressure of 0.04 Pa at 1400 K. Under plasma exposure deuterium capture in RG-Ti graphite reached the saturation level at a fluence of 4 x 10{sup 20} D/cm{sup 2} while the bulk inventory was negligible. As for POCO graphite, deuterium retention increased with fluence and was equal to 18 appm in the bulk for a fluence of 7 x 10{sup 21} D/cm{sup 2}. The same amount of deuterium in the bulk was obtained after gas exposure of POCO at an effective pressure of 0.8 Pa (1400 K, 6 h). With this result, the tritium concentration in the plasma-facing graphite materials can reach 1500 appm or 380 grams of tritium per ton of graphite. To understand the role of ion flux in generation of effective pressure, POCO was irradiated with 16 keV D{sub 2}{sup +}-ions at 1400 K for 4 h to 8 x 10{sup 20} D/cm{sup 2} (ion flux was 6 x 10{sup 16} D/cm{sup 2}.s, residual deuterium pressure was 0.004 Pa). The results are discussed on the basis of structural differences for POCO and RG-Ti graphites. (orig.).

  11. Modifications of Graphite and Multiwall Carbon Nanotubes in the Presence of Urea

    Science.gov (United States)

    Duraia, El-Shazly M.; Fahami, Abbas; Beall, Gary W.

    2018-02-01

    The effect of high-energy ball milling on two carbon allotropes, graphite and multiwall carbon nanotubes (MWCNT) in the presence of urea has been studied. Samples were investigated using Raman spectroscopy, x-ray diffraction, scanning electron microscope (SEM) and x-ray photoelectron spectroscopy (XPS). Nitrogen-doped graphene has been successfully synthesized via a simple scalable mechanochemistry method using urea and graphite powder precursors. XPS results revealed the existence of the different nitrogen atoms configurations including pyridine, pyrrodic and graphitic N. SEM observations showed that the graphene nanosheets morphology become more wrinkles folded and crumbled as the milling time increased. The ID/IG ratio also increased as the milling time rose. The presence of both D' and G + D bands at 1621 cm-1 and 2940 cm-1, respectively, demonstrated the nitrogen incorporation in the graphene lattice Two factors contribute to the used urea: first it helps to exfoliate graphite into graphene, and second it preserves the graphitic structure from damage during the milling process as well as acting as a solid-state nitrogen source. Based on the phase analysis, the d-spacing of MWCNT samples in the presence of urea decreased due to the mechanical force in the milling process as the milling time increased. On the other hand, in the graphite case, due to its open flat surface, the graphite (002) peak shifts toward lower two theta as the milling time increase. Such findings are important and could be used for large-scale production of N-doped graphene, diminishing the use of either dangerous chemicals or sophisticated equipment.

  12. Modifications of Graphite and Multiwall Carbon Nanotubes in the Presence of Urea

    Science.gov (United States)

    Duraia, El-Shazly M.; Fahami, Abbas; Beall, Gary W.

    2017-11-01

    The effect of high-energy ball milling on two carbon allotropes, graphite and multiwall carbon nanotubes (MWCNT) in the presence of urea has been studied. Samples were investigated using Raman spectroscopy, x-ray diffraction, scanning electron microscope (SEM) and x-ray photoelectron spectroscopy (XPS). Nitrogen-doped graphene has been successfully synthesized via a simple scalable mechanochemistry method using urea and graphite powder precursors. XPS results revealed the existence of the different nitrogen atoms configurations including pyridine, pyrrodic and graphitic N. SEM observations showed that the graphene nanosheets morphology become more wrinkles folded and crumbled as the milling time increased. The ID/IG ratio also increased as the milling time rose. The presence of both D' and G + D bands at 1621 cm-1 and 2940 cm-1, respectively, demonstrated the nitrogen incorporation in the graphene lattice Two factors contribute to the used urea: first it helps to exfoliate graphite into graphene, and second it preserves the graphitic structure from damage during the milling process as well as acting as a solid-state nitrogen source. Based on the phase analysis, the d-spacing of MWCNT samples in the presence of urea decreased due to the mechanical force in the milling process as the milling time increased. On the other hand, in the graphite case, due to its open flat surface, the graphite (002) peak shifts toward lower two theta as the milling time increase. Such findings are important and could be used for large-scale production of N-doped graphene, diminishing the use of either dangerous chemicals or sophisticated equipment.

  13. Establishing isokinetic flow for a plasma torch exhaust gas diagnostic for a plasma hearth furnace

    Energy Technology Data Exchange (ETDEWEB)

    Pollack, Brian R. [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States)

    1996-05-01

    Real time monitoring of toxic metallic effluents in confined gas streams can be accomplished through use of Microwave Induced Plasmas to perform atomic emission spectroscopy, For this diagnostic to be viable it is necessary that it sample from the flowstream of interest in an isokinetic manner. A method of isokinetic sampling was established for this device for use in the exhaust system of a plasma hearth vitrification furnace. The flow and entrained particulate environment were simulated in the laboratory setting using a variable flow duct of the same dimensions (8-inch diameter, schedule 40) as that in the field and was loaded with similar particulate (less than 10 μm in diameter) of lake bed soil typically used in the vitrification process. The flow from the furnace was assumed to be straight flow. To reproduce this effect a flow straightener was installed in the device. An isokinetic sampling train was designed to include the plasma torch, with microwave power input operating at 2.45 GHz, to match local freestream velocities between 800 and 2400 ft/sec. The isokinetic sampling system worked as planned and the plasma torch had no difficulty operating at the required flowrates. Simulation of the particulate suspension was also successful. Steady particle feeds were maintained over long periods of time and the plasma diagnostic responded as expected.

  14. A Physically-Based Equivalent Circuit Model for the Impedance of a LiFePO4/Graphite 26650 Cylindrical Cell

    DEFF Research Database (Denmark)

    Scipioni, Roberto; Jørgensen, Peter Stanley; Graves, Christopher R.

    2017-01-01

    In this work an Equivalent Circuit Model (ECM) is developed and used to model impedance spectra measured on a commercial 26650 LiFePO4/Graphite cylindrical cell. The ECM is based on measurements and modeling of impedance spectra recorded separately on cathode (LiFePO4) and anode (Graphite) sample...

  15. DUCT RETROFIT STRATEGY TO COMPLEMENT A MODULATING FURNACE.

    Energy Technology Data Exchange (ETDEWEB)

    ANDREWS,J.W.

    2002-10-02

    Some recent work (Walker 2001, Andrews 2002) has indicated that installing a modulating furnace in a conventional duct system may, in many cases, result in a significant degradation in thermal distribution efficiency. The fundamental mechanism was pointed out nearly two decades ago (Andrews and Krajewski 1985). The problem occurs in duct systems that are less-than-perfectly insulated (e.g., R-4 duct wrap) and are located outside the conditioned space. It stems from the fact that when the airflow rate is reduced, as it will be when the modulating furnace reduces its heat output rate, the supply air will have a longer residence time in the ducts and will therefore lose a greater percentage of its heat by conduction than it did at the higher airflow rate. The impact of duct leakage, on the other hand, is not expected to change very much under furnace modulation. The pressures in the duct system will be reduced when the airflow rate is reduced, thus reducing the leakage per unit time. This is balanced by the fact that the operating time will increase in order to meet the same heating load as with the conventional furnace operating at higher output and airflow rates. The balance would be exact if the exponent in the pressure vs. airflow equation were the same as that in the pressure vs. duct leakage equation. Since the pressure-airflow exponent is usually {approx}0.5 and the pressure-leakage exponent is usually {approx}0.6, the leakage loss as a fraction of the load should be slightly lower for the modulating furnace. The difference, however, is expected to be small, determined as it is by a function with an exponent equal to the difference between the above two exponents, or {approx}0.1. The negative impact of increased thermal conduction losses from the duct system may be partially offset by improved efficiency of the modulating furnace itself. Also, the modulating furnace will cycle on and off less often than a single-capacity model, and this may add a small amount

  16. Optimizing of Work Arc Furnace to Decopperisation of Flash Slag

    Directory of Open Access Journals (Sweden)

    Bydałek A.W.

    2015-09-01

    Full Text Available Discusses an attempt to optimize the operation of an electric furnace slag to be decopperisation suspension of the internal recycling process for the production of copper. The paper presents a new method to recover copper from metallurgical slags in arc-resistance electric furnace. It involves the use of alternating current for a first period reduction, constant or pulsed DC in the final stage of processing. Even distribution of the electric field density in the final phase of melting caused to achieve an extremely low content of metallic copper in the slag phase. They achieved by including the economic effects by reducing the time reduction.

  17. Secondary Aluminum Melting Research in a Laboratory Scale Reverberatory Furnace

    Energy Technology Data Exchange (ETDEWEB)

    Clark, J.A., III

    2003-01-01

    The Albany Research Center (ARC), U.S. Department of Energy, has developed a 175-pound capacity, natural gas, direct-fired reverberatory furnace. The high temperature reactions present during the aluminum remelt process are being investigated. Preventing dross formation has been the key aim to date. Reducing losses to dross by 25-50% will potentially lead to an annual energy savings of over 75 trillion BTU's by the year 2020. Schematics and operation characteristics of the ARC Laboratory Scale Reverberatory Furnace (LSRF) will be presented. Potential gas-solid, gas-liquid, and liquid-solid interactions between the hot combustion gases, aluminum, and refractories will be discussed.

  18. Modeling the Gas-Solid Flow in Calcining Furnace

    Directory of Open Access Journals (Sweden)

    Haiyan Luo

    2011-03-01

    Full Text Available Gas-solid two-phase flow in calcining furnace is investigated in this paper. The turbulent fluid phase is calculated using the RNG k-e two-equation model in the Eulerain framework while the solid phase being handled via the particle stochastic trajectory model is calculated in the Lagrangian framework. Flow pattern characteristics of the fluid phase and the particle trajectories of the solid phase were predicted subject to a range of flow conditions and different particle sizes. The computed results provided useful information in the preview of kinetics regulation of the gas-solid two-phase in calcining furnace.

  19. Effect of alkaline elements on the reactivity, strength and structural properties of blast furnace cokes

    Directory of Open Access Journals (Sweden)

    A. Bhattacharyya

    2015-07-01

    Full Text Available The present study concerns itself on the adverse effects of alkaline elements like sodium and potassium on blast furnace cokes. To achieve a deeper insight on the effects of alkaline elements on coke reactivity and strength, industrial coke samples impregnated with different alkaline species in various amounts have been tested under standard conditions to find out their Coke Reactivity Index (CRI and Coke Strength after Reaction (CSR values. Scanning electron microscopy, petrographic and Raman Spectrometric investigations demonstrate the change of structural properties. The mechanism of catalysis has been postulated.

  20. Total arsenic in urine: palladium-persulfate vs nickel as a matrix modifier for graphite furnace atomic absorption spectrophotometry.

    Science.gov (United States)

    Nixon, D E; Mussmann, G V; Eckdahl, S J; Moyer, T P

    1991-09-01

    We evaluated the effectiveness of nickel and palladium with or without added potassium persulfate as matrix modifiers for the determination of total arsenic in urine. Complete recovery of pure aqueous solutions of As(III), As(V), cacodylic acid (DMA), monomethylarsinic acid (MMA), and o-arsanilic acid was attained by using both nickel and palladium modifiers. Combined arsenobetaine and arsenocholine (so-called fish arsenic), extracted from a certified control material of dogfish muscle (DORM-1), were completely recovered with Pd-S2O8 matrix modification, but not with nickel. Excellent agreement with target values for arsenic in urines from the Centre de Toxicologie du Quebec, supplied by the Interlaboratory Comparison Program, was attained irrespective of the arsenic source when we used Pd-S2O8 as the matrix modifier.

  1. First principles study of oxidation behavior of irradiated graphite

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Juan; Dong, Limin [Beijing Key Lab of Fine Ceramics, Institute of Nuclear and New Energy Technology, Tsinghua University, Beijing 100084 (China); Wang, Chen [State Key Lab of New Ceramic and Fine Processing, Tsinghua University, Beijing 100084 (China); Liang, Tongxiang, E-mail: txliang@tsinghua.edu.cn [State Key Lab of New Ceramic and Fine Processing, Tsinghua University, Beijing 100084 (China); Lai, Wensheng [Advanced Material Laboratory, School of Materials Science & Engineering, Tsinghua University, Beijing 100084 (China)

    2015-06-01

    The relationship between nuclear graphite microstructure and its oxidation resistance underlines the importance of comprehensive oxidation characterization studies of the new grades of nuclear graphite. Periodic DFT calculations are performed to model oxidation behavior of irradiated graphite. O{sub 2} molecules adsorbed on perfect and defective graphite surfaces are calculated. The adsorptive energy of O{sub 2} on defective graphite adsorption site with one carbon atom missing is approximately 10 times as strong as that on a defect-free perfect graphite surface. Monovacancy and divacancy on graphite surface can easily chemisorb O{sub 2} molecule compared to perfect surface. Two oxidation processes including CO and CO{sub 2} formation steps are analyzed. For symmetric monovacancy defect, three dangling C atoms are unsaturated and exhibit high adsorption ability, as well as reconstructed monovacancy and divacancy defects. These vacancy defects in irradiated graphite decrease oxidation resistance of nuclear graphite.

  2. Heat and mass transfer in a vertical flue ring furnace

    Energy Technology Data Exchange (ETDEWEB)

    Jacobsen, Mona

    1997-12-31

    The main emphasis of this thesis was the design of a mathematical simulation model for studying details in the baking of anodes in the Hydro Aluminium anode baking furnace. The change of thermal conductivity, density, porosity and permeability during heat treatment was investigated. The Transient Plane Source technique for measuring thermal conductivity of solids was used on green carbon materials during the baking process in the temperature range 20-600 {sup o}C. Next, change of mass, density, porosity and permeability of anode samples were measured after being baked to temperatures between 300 and 1200 {sup o}C. The experimental data were used for parameter estimation and verification of property models for use in the anode baking models. Two distinct mathematical models have been modified to study the anode baking. A transient one-dimensional model for studying temperature, pressure and gas evolution in porous anodes during baking was developed. This was extended to a two-dimensional model incorporating the flue gas flow. The mathematical model which included porous heat and mass transfer, pitch pyrolysis, combustion of volatiles, radiation and turbulent channel flow, was developed by source code modification of the Computational Fluid Dynamics code FLUENT. The two-dimensional geometry of a flue gas channel adjacent to a porous flue gas wall, packing coke and anode was used for studying the effect of different firing strategies, raw materials properties and packing coke thickness. The model proved useful for studying the effects of heating rate, geometry and anode properties. 152 refs., 73 figs, 11 tabs.

  3. Graphene prepared by thermal reduction–exfoliation of graphite oxide: Effect of raw graphite particle size on the properties of graphite oxide and graphene

    Energy Technology Data Exchange (ETDEWEB)

    Dao, Trung Dung; Jeong, Han Mo, E-mail: hmjeong@mail.ulsan.ac.kr

    2015-10-15

    Highlights: • Effect of raw graphite particle size on properties of GO and graphene is reported. • Size of raw graphite affects oxidation degree and chemical structure of GO. • Highly oxidized GO results in small-sized but well-exfoliated graphene. • GO properties affect reduction degree, structure, and conductivity of graphene. - Abstract: We report the effect of raw graphite size on the properties of graphite oxide and graphene prepared by thermal reduction–exfoliation of graphite oxide. Transmission electron microscope analysis shows that the lateral size of graphene becomes smaller when smaller size graphite is used. X-ray diffraction analysis confirms that graphite with smaller size is more effectively oxidized, resulting in a more effective subsequent exfoliation of the obtained graphite oxide toward graphene. X-ray photoelectron spectroscopy demonstrates that reduction of the graphite oxide derived from smaller size graphite into graphene is more efficient. However, Raman analysis suggests that the average size of the in-plane sp{sup 2}-carbon domains on graphene is smaller when smaller size graphite is used. The enhanced reduction degree and the reduced size of sp{sup 2}-carbon domains contribute contradictively to the electrical conductivity of graphene when the particle size of raw graphite reduces.

  4. Possible room temperature superconductivity in conductors obtained by bringing alkanes into contact with a graphite surface

    Science.gov (United States)

    Kawashima, Yasushi

    2013-05-01

    Electrical resistances of conductors obtained by bringing alkanes into contact with a graphite surface have been investigated at room temperatures. Ring current in a ring-shaped container into which n-octane-soaked thin graphite flakes were compressed did not decay for 50 days at room temperature. After two HOPG plates were immersed into n-heptane and n-octane at room temperature, changes in resistances of the two samples were measured by four terminal technique. The measurement showed that the resistances of these samples decrease to less than the smallest resistance that can be measured with a high resolution digital voltmeter (0.1μV). The observation of persistent currents in the ring-shaped container suggests that the HOPG plates immersed in n-heptane and n-octane really entered zero-resistance state at room temperature. These results suggest that room temperature superconductor may be obtained by bringing alkanes into contact with a graphite surface.

  5. Resistivity of pristine and intercalated graphite fiber epoxy composites

    Science.gov (United States)

    Gaier, James R.; Hambourger, Paul D.; Slabe, Melissa E.

    1991-01-01

    Laminar composites were fabricated from pristine and bromine intercalated Amoco P-55, P-75, and P-100 graphite fibers and Hysol-Grafil EAG101-1 film epoxy. The thickness and r.f. eddy current resistivity of several samples were measured at grid points and averaged point by point to obtain final values. Although the values obtained this way have high precision (less than 3 percent deviation), the resistivity values appear to be 20 to 90 percent higher than resistivities measured on high aspect ratio samples using multi-point techniques, and by those predicted by theory. The temperature dependence of the resistivity indicates that the fibers are neither damaged nor deintercalated by the composite fabrication process. The resistivity of the composites is a function of sample thickness (i.e., resin content). Composite resistivity is dominated by fiber resistivity, so lowering the resistivity of the fibers, either through increased graphitization or intercalation, results in a lower composite resistivity. A modification of the simple rule of mixtures model appears to predict the conductivity of high aspect ratio samples measured along a fiber direction, but a directional dependence appears which is not predicted by the theory. The resistivity of these materials is clearly more complex than that of homogeneous materials.

  6. Studies of mechanical properties and irradiation damage nucleation of HTGR graphites. Progress report, February 1, 1976--January 31, 1977. [2020 and H440 graphites

    Energy Technology Data Exchange (ETDEWEB)

    Thrower, P.A.

    1977-02-01

    Sample preparation for irradiation studies was completed, but irradiations are unlikely to commence until late 1977. The effect of compressive stresses up to 650 psi on the reaction rate of Stackpole 2020 graphite with helium containing small amounts of either H/sub 2/O or CO/sub 2/ was investigated. In no case was any effect found. Relationships between the compressive strengths of 2020 and Great Lakes H440 graphites and air oxidation burn-off show that a 10% burn-off results in a 50% strength reduction. Sample external dimensions were unchanged even with a 50% burn-off. Strain to failure was relatively independent of burn-off except for 2020 graphite with burn-offs in excess of approximately 28%, when strains increased rapidly. Scanning electron microscope examination reveals preferential removal of binder material over filler particles. The effect of flow rate of He/H/sub 2/O and He/CO/sub 2/ gas mixtures over the graphite sample during oxidation showed a decrease in oxidation rate with increasing flow rate in the flow range 13.8 to 15.3 ml/s. 9 figures, 2 tables.

  7. Nonlinear optical characterization of graphite oxide thin film by open aperture Z-scan technique

    Energy Technology Data Exchange (ETDEWEB)

    Sreeja, V. G.; Reshmi, R.; Devasia, Sebin; Anila, E. I., E-mail: anilaei@gmail.com [Optolectronic and Nanomaterials Research Laboratory, Department of Physics, Union Christian College, Aluva-683 102, Kerala (India); Cheruvalathu, Ajina [International School of Photonics, CUSAT, Cochin-22 (India)

    2016-05-23

    In this paper we explore the structural characterization of graphite oxide powder prepared from graphite powder by oxidation via modified Hummers method. The nonlinear optical properties of the spin coated graphite oxide thin film is also explored by open aperture Z-Scan technique. Structural and physiochemical properties of the samples were investigated with the help of Fourier Transform Infrared Spectroscopy (FTIR) and Raman Spectroscopy (Raman).The results of FT-IR and Raman spectroscopy showed that the graphite is oxidized by strong oxidants and the oxygen atoms are introduced into the graphite layers forming C=C, O-H and –C-H groups. The synthesized sample has good crystalline nature with lesser defects. The nonlinear optical property of GO thin film was studied by open aperture Z-Scan technique using Q-switched Nd-Yag Laser at 532 nm. The Z-scan plot showed that the investigated GO thin film has saturable absorption behavior. The nonlinear absorption coefficient and saturation intensity were also estimated to explore its applications in Q switched mode locking laser systems.

  8. Influence of boron on ferrite formation in copper-added spheroidal graphite cast iron

    Directory of Open Access Journals (Sweden)

    Ying Zou

    2014-07-01

    Full Text Available This paper reviews the original work of the authors published recently, describing the influence of B on the matrix of the Cuadded spheroidal graphite cast iron. The effect of Cu has been corrected as a ferrite formation promoter in the matrix of the grey cast iron by the usage of high-purity material. Also, this paper focuses on the ferrite formation and the observation of the Cu distribution in the B-added and B-free Cu-containing spheroidal graphite cast iron. The Cu film on the spheroidal graphite can be successfully observed in the B-free sample using a special etching method. However, in the B-added sample, no Cu film could be found, while the secondary graphite was formed on the surface of the spheroidal graphite. The interaction between B and Cu is stressed as a peculiar phenomenon by the employment of a contrast experiment of B and Mn. The heat treatment could make Cu precipitate more significantly in the eutectic cells and in the matrix in the form of large Cu particles because of the limited solubility of Cu.

  9. Method of producing exfoliated graphite, flexible graphite, and nano-scaled graphene platelets

    Science.gov (United States)

    Zhamu, Aruna; Shi, Jinjun; Guo, Jiusheng; Jang, Bor Z.

    2010-11-02

    The present invention provides a method of exfoliating a layered material (e.g., graphite and graphite oxide) to produce nano-scaled platelets having a thickness smaller than 100 nm, typically smaller than 10 nm. The method comprises (a) dispersing particles of graphite, graphite oxide, or a non-graphite laminar compound in a liquid medium containing therein a surfactant or dispersing agent to obtain a stable suspension or slurry; and (b) exposing the suspension or slurry to ultrasonic waves at an energy level for a sufficient length of time to produce separated nano-scaled platelets. The nano-scaled platelets are candidate reinforcement fillers for polymer nanocomposites. Nano-scaled graphene platelets are much lower-cost alternatives to carbon nano-tubes or carbon nano-fibers.

  10. Graphite matrix materials for nuclear waste isolation

    Energy Technology Data Exchange (ETDEWEB)

    Morgan, W.C.

    1981-06-01

    At low temperatures, graphites are chemically inert to all but the strongest oxidizing agents. The raw materials from which artificial graphites are produced are plentiful and inexpensive. Morover, the physical properties of artificial graphites can be varied over a very wide range by the choice of raw materials and manufacturing processes. Manufacturing processes are reviewed herein, with primary emphasis on those processes which might be used to produce a graphite matrix for the waste forms. The approach, recommended herein, involves the low-temperature compaction of a finely ground powder produced from graphitized petroleum coke. The resultant compacts should have fairly good strength, low permeability to both liquids and gases, and anisotropic physical properties. In particular, the anisotropy of the thermal expansion coefficients and the thermal conductivity should be advantageous for this application. With two possible exceptions, the graphite matrix appears to be superior to the metal alloy matrices which have been recommended in prior studies. The two possible exceptions are the requirements on strength and permeability; both requirements will be strongly influenced by the containment design, including the choice of materials and the waste form, of the multibarrier package. Various methods for increasing the strength, and for decreasing the permeability of the matrix, are reviewed and discussed in the sections in Incorporation of Other Materials and Elimination of Porosity. However, it would be premature to recommend a particular process until the overall multi-barrier design is better defined. It is recommended that increased emphasis be placed on further development of the low-temperature compacted graphite matrix concept.

  11. The determination of the content of gold and silver in geological samples

    Directory of Open Access Journals (Sweden)

    B. NESIC

    2001-01-01

    Full Text Available A method has been elaborated for the determination of the content of gold and silver in geological samples by atomic absorption spectrophotometry (AAS in combination with the fire assay method. The weight of sample used for analysis was 10 g. Sulphur present as sulphide, which is an undesirable element in smelting, was removed by the addition of iron to the charge. The sample was smelted with fluxes and lead oxide to replace the silver and gold by lead and to transfer non-precious elements to slag. Lead was separated from precious metals by cupellation. The separated silver and gold alloy was dissolved with aqua regia with addition of hydrochloric acid in excess. Silver and gold were determined from the same solution. For determination of the silver content, the AAS method with an air-acetylene flame was used. Gold was determined in a graphite furnace with the addition of a matrix modifier in an argon current, at an atomization temperature of t = 2200°C. The lower determination limit for silver was 0.05 g/t and for gold 0.005 g/t. The results of the analysis for silver and gold obtained with the proposed method showed good agreement with the results of the analysis of the same samples with the fire assay method.

  12. Method of fabricating silicon carbide coatings on graphite surfaces

    Science.gov (United States)

    Varacalle, D.J. Jr.; Herman, H.; Burchell, T.D.

    1994-07-26

    The vacuum plasma spray process produces well-bonded, dense, stress-free coatings for a variety of materials on a wide range of substrates. The process is used in many industries to provide for the excellent wear, corrosion resistance, and high temperature behavior of the fabricated coatings. In this application, silicon metal is deposited on graphite. This invention discloses the optimum processing parameters for as-sprayed coating qualities. The method also discloses the effect of thermal cycling on silicon samples in an inert helium atmosphere at about 1,600 C which transforms the coating to silicon carbide. 3 figs.

  13. Solvation and squeeze out of hexadecane on graphite

    Science.gov (United States)

    Gosvami, N. N.; Sinha, S. K.; Hofbauer, W.; O'Shea, S. J.

    2007-06-01

    We have performed simultaneous force and conductivity measurement of hexadecane liquid confined between a conducting atomic force microscope tip and a graphite surface. Both the current and the force data reveal discrete solvation layering of the hexadecane near the surface. We typically observe that the current does not vary with load in a simple way as the layer closest to the surface is compressed, but increases markedly prior to the expulsion of material from the tip-sample gap. We infer that even for a nanoscale asperity there is conformation change of the confined hexadecane under the tip apex prior to squeeze out of the molecules.

  14. Fracture toughness of graphite composites

    Energy Technology Data Exchange (ETDEWEB)

    Blikstad, M.

    1985-01-01

    The first two papers in the thesis deal with moisture absorption in graphite/epoxy materials. Both one- and three-dimensional moisture absoption were studied. The diffusion along the fiber direction was measured. A great difference was found between the diffusion along the fiber direction and the diffusion perpendicular to the fiber direction. The experimental results were compared with three-dimensional calculations based on Fick's second law of diffusion. Edge delamination is the main subject of the next two papers. Angle-ply specimens with standard and toughened resin were loaded in tension before and after moisture absorption to obtain the fracture toughness for edge delamination. The mode of loading for inherent cracks along the edge in these types of specimens is essentially a combination of mode I and Mode III. The delamination fracture surfaces were studied in a scanning electron microscope (SEM). They exhibited hackle formation and the tilt of the hackles was found to be characteristic of the state of stress in the interlaminar region. The obtained fracture toughnesses were analyzed according to the geometrical fracture criterion. Change to a more ductile epoxy resin increased the fracture toughness. In the fifth paper the fracture toughness of ply cracking was measured in unidirectional off-axis and rail shear test specimens. By varying the off-axis angle the mode of loading was varied from pure mode I to nearly mode II. The rail shear test gave pure mode II loading. The fracture surfaces were investigated in a SEM. The obtained fracture toughness was analyzed according to the quadratic mixed mode fracture criterion. Moisturizatio of the standard resin laminate and change to a more ductile epoxy resin increased the fracture toughness. However, when the toughened resin laminate had absorbed moisture, its toughness decreased substantially.

  15. Computational fluid dynamics simulations of a glass melting furnace

    Energy Technology Data Exchange (ETDEWEB)

    Egelja, A.; Lottes, S. A.

    2000-05-09

    The glass production industry is one of the major users of natural gas in the US, and approximately 75% of the energy produced from natural gas is used in the melting process. Industrial scale glass melting furnaces are large devices, typically 5 or more meters wide, and twice as long. To achieve efficient heat transfer to the glass melt below, the natural gas flame must extend over a large portion of the glass melt. Therefore modern high efficiency burners are not used in these furnaces. The natural gas is injected as a jet, and a jet flame forms in the flow of air entering the furnace. In most current glass furnaces the energy required to melt the batch feed stock is about twice the theoretical requirement. An improved understanding of the heat transfer and two phase flow processes in the glass melt and solid batch mix offers a substantial opportunity for energy savings and consequent emission reductions. The batch coverage form and the heat flux distribution have a strong influence on the glass flow pattern. This flow pattern determines to a significant extent the melting rate and the quality of glass.

  16. Heuristic algorithms for scheduling heat-treatment furnaces of steel ...

    Indian Academy of Sciences (India)

    treatment furnaces in a steel-casting foundry, a special problem of batch processor scheduling, ... production management is to maximize throughput and reduce flow time and WIP. This motivated the choice of ..... A computational experiment is appropriate in order to provide a perspective on the relative effectiveness of any ...

  17. Optimization of burners in oxygen-gas fired glass furnace

    NARCIS (Netherlands)

    Kersbergen, M.J. van; Beerkens, R.G.C.; Sarmiento-Darkin, W.; Kobayashi, H.

    2012-01-01

    The energy efficiency performance, production stability and emissions of oxygen-fired glass furnaces are influenced by the type of burner, burner nozzle sizes, burner positions, burner settings, oxygen-gas ratios and the fuel distribution among all the burners. These parameters have been optimized

  18. Analysis of combustion efficiency in a pelletizing furnace

    Directory of Open Access Journals (Sweden)

    Rafael Simões Vieira de Moura

    Full Text Available Abstract The objective of this research is to assess how much the improvement in the combustion reaction efficiency can reduce fuel consumption, maintaining the same thermal energy rate provided by the reaction in a pelletizing furnace. The furnace for pelletizing iron ore is a complex thermal machine, in terms of energy balance. It contains recirculation fan gases and constant variations in the process, and the variation of a single process variable can influence numerous changes in operating conditions. This study demonstrated how the main variables related to combustion in the burning zone influence fuel consumption (natural gas from the furnace of the Usina de Pelotização de Fábrica (owned by VALE S/A, without changing process conditions that affect production quality. Variables were analyzed regarding the velocity and pressure of the fuel in the burners, the temperature of the combustion air and reactant gases, the conversion rate and the stoichiometric air/fuel ratio of the reaction. For the analysis, actual data of the furnace in operation was used, and for the simulation of chemical reactions, the software Gaseq® was used. The study showed that the adjustment of combustion reaction stoichiometry provides a reduction of 9.25% in fuel consumption, representing a savings of US$ 2.6 million per year for the company.

  19. Chloride ingress of carbonated blast furnace slag cement mortars

    NARCIS (Netherlands)

    Holthuizen, P.E.; Çopuroglu, O.; Polder, R.B.

    2017-01-01

    In the Netherlands civil engineering structures, such as overpasses, bridges and tunnels are generally built using blast furnace slag cement (BFSC, CEM III/B) concrete, because of its high resistance against chloride penetration. Although the Dutch experience regarding durability performance of BFSC

  20. Heuristic algorithms for scheduling heat-treatment furnaces of steel ...

    Indian Academy of Sciences (India)

    The scheduling of furnaces for heat-treatment of castings is of considerable interest as a large proportion of the total production time is the processing times of these ... Department of Management Studies, Indian Institute of Science, Bangalore 560 012; Singapore-MIT Alliance, School of Mechanical and Aerospace ...