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

    International Nuclear Information System (INIS)

    Bentlin, Fabrina R.S.; Pozebon, Dirce; Mello, Paola A.; Flores, Erico M.M.

    2007-01-01

    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 3 ) 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 μg g -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)

  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. Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2015-03-01

    The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%). - Highlights: • High-resolution Graphite Furnace Molecular Absorption Spectrometry (HR-GF MAS) • Fluorine has been determined using HR-GF MAS of the CaF molecule. • The CaF molecule was generated in a graphite furnace at a temperature of 2100 °C • Coal samples have been analyzed using direct solid sample introduction. • Aqueous standard solutions have been used for calibration.

  5. Determination of arsenic and cadmium in shellfish samples by graphite furnace atomic absorption spectrometry using matrix modifier

    International Nuclear Information System (INIS)

    Cortez Diaz, Mirella del Carmen

    2002-01-01

    Heavy metals are a big source of environmental contamination and are also highly toxic to humans. Since shellfish are bio-accumulators of these metals, proper techniques for quantifying them should be available. This work aims to develop an analytical method for the quantitative determination of heavy metals in biological materials (shellfish), specifically arsenic and cadmium at the trace level, using graphite furnace atomic absorption spectrometry, for which nickel and phosphate solutions were used to modify the modifiers. Prior to the analysis, the sample was diluted with nitric acid in a DAB II pressure digestion system order to destroy the organic matter. The instrument conditions were initially set (wavelength, slit, integration peaks, graphite tube, etc.), then the work range was defined for each element and the most appropriate operational parameters were studied, such as: temperature, ramp times, hold times and internal gas flow, in the different stage of the electrothermal treatment (drying, calcination, atomization) for the furnace program. Once the above mentioned conditions were set and since this was a biological sample, a matrix chemical modifier had to be used, in order to make the elements that accompany the element being studied more volatile. In this way the chemical and spectral interferences decrease together with the high background absorption of the matrix. Therefore, different matrix modifiers were studied for the definition of each analyte. The method validation was done using Certified Oyster Tissue Reference Material N o 1566a from the National Institute of Standards and Technology applying different tests in order to eliminate outliers. Repeatability, uncertainty, sensitivity, lineal range, working range, detection limit and quantification limit were evaluated for each element, and the results were compared with the values for the certified material. The Fisher and Student tests were the statistical tools used. The experimental values

  6. Solid sampling-graphite furnace atomic absorption spectrometry for the direct determination of boron in plant tissues

    International Nuclear Information System (INIS)

    Resano, M.; Briceno, J.; Aramendia, M.; Belarra, M.A.

    2007-01-01

    In this work, the potential of graphite furnace atomic absorption spectrometry for the direct determination of B in plant tissues has been investigated. Three certified reference materials (NIST SRM 1570a spinach leaves, NIST SRM 1573a tomato leaves and BCR CRM 679 white cabbage) were selected for this study, the goal always being to develop a fast procedure that could be robust enough to provide a satisfactory performance for all of them, without any modifications in the conditions applied. The use of a suitable chemical modifier was found to be essential for obtaining a reproducible and sufficiently sensitive signal for boron solutions. In this regard, the performance of the combination of citric acid plus W (added as a permanent modifier) was noteworthy, resulting in well-defined signal profiles, a remarkable analyte stabilization during the pyrolysis step (up to 2100 deg. C) and minimal memory effects. This mixture of modifiers provided a good performance for the direct analysis of solid samples as well, but only if a suitable temperature program, favoring the interaction between the analyte and the modifiers, was used. Thus, such a temperature program, with two pyrolysis steps and the addition of NH 4 NO 3 in order to carry out the in situ sample microdigestion, was optimized. Under these conditions, the peak areas obtained for both solid samples and aqueous standards were comparable. Finally, the analysis of the samples was carried out. In all cases, a good agreement with the certified values was obtained, while R.S.D. values ranged between 6 and 10%. It can be concluded that the method proposed shows significant advantages for the determination of this complicated element in solid samples such as the use of aqueous standards for calibration, a high sample throughput (20 min per sample), a suitable limit of detection (0.3 μg g -1 ) and reduced risk of analyte losses and contamination

  7. Determination of gold and cobalt dopants in advanced materials based on tin oxide by slurry sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Filatova, Daria G.; Eskina, Vasilina V.; Baranovskaya, Vasilisa B.; Vladimirova, Svetlana A.; Gaskov, Alexander M.; Rumyantseva, Marina N.; Karpov, Yuri A.

    2018-02-01

    A novel approach is developed for the determination of Co and Au dopants in advanced materials based on tin oxide using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) with direct slurry sampling. Sodium carboxylmethylcellulose (Na-CMC) is an effective stabilizer for diluted suspensions. Use Na-CMC allows to transfer the analytes into graphite furnace completely and reproducibly. The relative standard deviation obtained by HR CS GFAAS was not higher than 4%. Accuracy was proven by means inductively coupled plasma mass spectrometry (ICP-MS) in solutions after decomposition as a comparative technique. To determine Au and Co in the volume of SnO2, the acid decomposition conditions (HCl, HF) of the samples were suggested by means of an autoclave in a microwave oven.

  8. Determination of arsenic and cadmium in shellfish samples by graphite furnace atomic absorption spectrometry using matrix modifier

    International Nuclear Information System (INIS)

    Villalobos Aranda, Juan; Cortez Diaz, Mirella

    2003-01-01

    Serious problems of environmental contamination due to the activity of the man exist at the present time. Where the greater impact is the produced one by heavy metals that go to the sea. Where the shellfish can collect some of them, the highly toxic ones, since these are bioaccumulation of these metals. Therefore one becomes necessary to count with the reliable analytical procedures to determine these elements. The purpose of this work is to present the determination of arsenic and cadmium in shellfish, by spectroscopy of atomic absorption with graphite furnace. For each determined element, solutions of nickel and phosphate like matrix modifiers were used respectively The validation was made using a Reference Certified Material, Oyster ' Tissue 156 (National Institute of Standards and Technology). The sample previously was digested in triplicate by two consecutive days, with nitric acid in a pressure digestion system DAB 11. For each element it was evaluated: limit of detection and quantification, sensitivity, repeatability, linear, slope rank and uncertainty. In addition, the obtained results were compared with the certified values of the certified material of reference using like statistical tools the tests of Student and Fisher. In both tests the calculated values were smaller to the shown ones in table, for degrees of freedom with 95% of confidence. Thus it was verified that it does not exist significant differences between the precision and the average values of the results obtained with respect to the values of the certified material. In addition, the obtained parameters are appropriate for the determination of these trace elements in this type of environmental sample (author)

  9. Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

    International Nuclear Information System (INIS)

    Ribeiro, Anderson Schwingel; Vieira, Mariana Antunes; Furtado da Silva, Alessandra; Borges, Daniel L. Gallindo; Welz, Bernhard; Heitmann, Uwe; Curtius, Adilson Jose

    2005-01-01

    Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 deg. C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 deg. C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g -1

  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 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.

  12. 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

  13. Feasibility of using in situ fusion for the determination of Co, Cr and Mn in Portland cement by direct solid sampling graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Intima, Danielle Polidorio; de Oliveira, Elisabeth; Oliveira, Pedro Vitoriano

    2009-01-01

    In situ fusion on the boat-type graphite platform has been used as a sample pretreatment for the direct determination of Co, Cr and Mn in Portland cement by solid sampling graphite furnace atomic absorption spectrometry (SS-GF AAS). The 3-field Zeeman technique was adopted for background correction to decrease the sensitivity during measurements. This strategy allowed working with up to 200 μg of sample. The in situ fusion was accomplished using 10 μL of a flux mixture 4.0% m/v Na 2 CO 3 + 4.0% m/v ZnO + 0.1% m/v Triton (registered) X-100 added over the cement sample and heated at 800 deg. C for 20 s. The resulting mould was completely dissolved with 10 μL of 0.1% m/v HNO 3 . Limits of detection were 0.11 μg g - 1 for Co, 1.1 μg g - 1 for Cr and 1.9 μg g - 1 for Mn. The accuracy of the proposed method has been evaluated by the analysis of certified reference materials. The values found presented no statistically significant differences compared to the certified values (Student's t-test, p < 0.05). In general, the relative standard deviation was lower than 12% (n = 5).

  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. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

    International Nuclear Information System (INIS)

    Matos Reyes, Mariela N.; Campos, Reinaldo C.

    2005-01-01

    A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO 3 at a 3.3:6.5:1 volume ratio. For Pb, efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier. The drying temperature and ramp rate influenced the sensitivity obtained for Ni, and had to be carefully optimized. Taking this into account, the same sensitivity was attained in all investigated organic media stabilized as microemulsion. Thus, calibration with microemulsions prepared with a single organic solvent was possible, using aqueous or organic stock solutions. Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures. n-Hexane microemulsions were used for calibration, and good agreement was obtained between the results using the proposed and comparative procedures. Typical coefficients of variation (n = 6) ranged from 1% to 4%, and from 1% to 3% for Ni and Pb, respectively. Detection limits (k = 3) in the original gasoline or diesel samples, derived from 10 blank measurements, were 4.5 and 3.6 μg l -1 for Ni and Pb, respectively, comfortably below the values found in the analyzed samples

  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 phospholipids in soybean lecithin samples via the phosphorus monoxide molecule by high-resolution continuum source graphite furnace molecular absorption spectrometry.

    Science.gov (United States)

    Pires, Laís N; Brandão, Geovani C; Teixeira, Leonardo S G

    2017-06-15

    This paper presents a method for determining phospholipids in soybean lecithin samples by phosphorus determination using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) via molecular absorption of phosphorus monoxide. Samples were diluted in methyl isobutyl ketone. The best conditions were found to be 213.561nm with a pyrolysis temperature of 1300°C, a volatilization temperature of 2300°C and Mg as a chemical modifier. To increase the analytical sensitivity, measurement of the absorbance signal was obtained by summing molecular transition lines for PO surrounding 213nm: 213.561, 213.526, 213.617 and 213.637nm. The limit of detection was 2.35mgg -1 and the precision, evaluated as relative standard deviation (RSD), was 2.47% (n=10) for a sample containing 2.2% (w/v) phosphorus. The developed method was applied for the analysis of commercial samples of soybean lecithin. The determined concentrations of phospholipids in the samples varied between 38.1 and 45% (w/v). Copyright © 2017 Elsevier Ltd. All rights reserved.

  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

    International Nuclear Information System (INIS)

    Virgilio, Alex; Nóbrega, Joaquim A.; Rêgo, Jardes F.; Neto, José A. Gomes

    2012-01-01

    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 °C and 2400 °C, respectively. Slopes of calibration curves (50–750 pg Cr, R 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 μg g −1 Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 ± 2.1 μg g −1 Cr. The limit of detection was 3.3 ng g −1 Cr. - Highlights: ► Direct solid sampling is first time employed for Cr in plant materials. ► Calibration curves with liquids and solids are coincident. ► Microanalysis of plants for Cr is validated by reference materials. ► The proposed HR-CS GF AAS method is environmental friendly.

  20. 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.

  1. 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.

  2. Strontium mono-chloride — A new molecule for the determination of chlorine using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Lopez, Alfredo H.D.; Gois, Jefferson S. de; Caramori, Giovanni F. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Borges, Daniel L.G.; Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2014-12-01

    A new method has been developed for the determination of chlorine in biological reference materials using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) of the strontium mono-chloride (SrCl) molecule and direct solid sample analysis. The use of the SrCl molecule for high-temperature MAS was not described up to now in the literature. Preliminary time-dependent density functional theory calculations of the SrCl structure were carried out in order to obtain reasonable estimates of the absorption spectrum of the target molecule. The calculations, which were carried out at BHandHLyp/def2-QZVP level of theory, proved a very accurate and inexpensive way to get information about the spectrum of the SrCl molecule, which enabled us to perform the Cl determination with good sensitivity and specificity. The molecular absorption of the SrCl molecule has been measured using the wavelength at 635.862 nm, and zirconium and palladium have been evaluated as the chemical modifiers in order to increase the sensitivity of the gaseous SrCl molecule generated in the graphite furnace. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Accuracy and precision of the method have been evaluated using biological certified reference materials of both animal and plant origins, showing good agreement with the informed and certified values. Limit of detection and characteristic mass were 1.0 and 2.2 ng, respectively. The results found using HR-CS GF MAS were in agreement (95% confidence level) compared to those obtained by electrothermal vaporization-inductively coupled plasma mass spectrometry. - Highlights: • The spectrum of the SrCl molecule was calculated on a theoretical basis and found very close to the predicted wavelength. • It is the first time that the spectrum of the SrCl molecule is described and used analytically for the determination of Cl. • No spectral interferences were observed as the

  3. 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.

  4. 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.

  5. Determination of tellurium in coal samples by means of graphite furnace atomic absorption spectrometry after coprecipitation with iron(III) hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Oda, S.; Arikawa, Y. [Japan Womens University, Tokyo (Japan)

    2005-11-01

    A simple and accurate method for the determination of tellurium in coal samples was investigated by the combustion of samples under a high pressure of oxygen and coprecipitation with Fe(OH){sub 3}, followed by a measurement by graphite furnace atomic absorption spectrometry (GF-AAS). About 0.5 g of an accurately weighed ground coal sample and 0.5 g of starch were combusted in an oxygen combustion bomb filled with oxygen to 3 MPa and added with 3 ml of water as an absorbing solution. The formed tellurium trioxide TeOs dissolved in water as TeO{sub 4}{sup 2-}, which was in turn reduced to TeO{sub 3}{sup 2-} by heating. After diluting the above-mentioned solution up to about 50 ml with water, Fe(OH){sub 3} is formed upon adding Fe(NO{sub 3}){sub 3} and sodium hydroxide solutions at pH 8-9 and left standing overnight. After dissolving the precipitate by HCl, the solution was diluted to 10 ml with water and the concentration of tellurium was measured by GF-AAS at a wavelength of 214.3 nm. The standard addition method was employed for the determination of tellurium in real coal samples, because those processes for the formation of tellurium(VI) oxide and coprecipitation with Fe(OH)3 were interfered by matrices. For NIST SRM 1632c, the standard coal sample tellurium content of 0.057 {+-} 0.004 mg kg{sup -1} was in good agreement with the information value of 0.05 mg kg{sup -1} with 7% of RSD in five replicate analyses. The tellurium contents in 20 real coal samples given by Center for Coal Utilization, Japan were also determined. The tellurium contents in these samples were scattered over the narrow range between 0.032 and 0.100 mg kg{sup -1}.

  6. Influence of citric acid as chemical modifier for lead determination in dietary calcium supplement samples by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Cezar Paz de Mattos, Julio; Medeiros Nunes, Adriane; Figueiredo Martins, Ayrton; Luiz Dressler, Valderi; Marlon de Moraes Flores, Erico

    2005-01-01

    Citric acid was used as a chemical modifier for Pb determination by graphite furnace atomic absorption spectrometry in dietary supplement samples (calcium carbonate, dolomite and oyster shell samples) and its efficiency was compared to the use of palladium. Pyrolysis and atomization curves were established without use of chemical modifier, with the addition of 20, 100 and 200 μg of citric acid, and with 3 μg of palladium. The citric acid modifier made possible the interference-free Pb determination in the presence of high concentrations of Ca and Mg nitrates. Acid sample digestion involving closed vessels (microwave-assisted and conventional heating) and acid attack using polypropylene vessels at room temperature were compared. All digestion procedures presented similar results for calcium carbonate and dolomite samples. However, for oyster shell samples accurate results were obtained only with the use of closed vessel systems. Analyte addition and matrix-matched standards were used for calibration. The characteristic mass for Pb using citric acid and palladium were 16 and 25 pg, respectively. The relative standard deviation (RSD) was always less than 5% when citric acid was used. The relative and absolute limits of detection were 0.02 μg g -1 and 8 pg with citric acid and 0.1 μg g -1 and 44 pg with the Pd modifier, respectively (n = 10, 3σ). The recovery of Pb in spiked calcium supplement samples (10 μg l -1 ) was between 98% and 105%. With the use of 100 μg of citric acid as chemical modifier, problems such as high background absorption and high RSD values were minimized in comparison to the addition of 3 μg of palladium

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

    African Journals Online (AJOL)

    spectrometry as alternative method for trace analysis of ... Purpose: To evaluate the comparative efficiency of graphite furnace atomic absorption spectrometry .... Methods comparison and validation .... plasma-optical emission spectrometry.

  8. Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

    2015-12-01

    The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

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

    International Nuclear Information System (INIS)

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

    2011-01-01

    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.

  10. 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.

  11. 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.

  12. Development of synthetic graphite resistive elements for sintering furnace

    International Nuclear Information System (INIS)

    Otani, C.; Rezende, Mirabel C.; Polidoro, H.A.; Otani, S.

    1987-01-01

    The synthetic graphites have been produced using lignin coke, natural graphite and phenolic resin. The bulk density, porosity, flexural strength and eletrical resistivity measurements have been performed on specimens at about 2400 0 C. The performance of these materials, as heating elements, was evaluated in a sintering furnace prototype. This paper reports the fabrication process and the experimental results. (Author) [pt

  13. Determination of fluorine in copper concentrate via high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis - Comparison of three target molecules.

    Science.gov (United States)

    Cadorim, Heloisa R; de Gois, Jefferson S; Borges, Aline R; Vale, Maria Goreti R; Welz, Bernhard; Gleisner, Heike; Ott, Christina

    2018-01-01

    The chemical composition of complex inorganic materials, such as copper concentrate, may influence the economics of their further processing because most smelters, and particularly the producers of high-purity electrolyte copper, have strict limitations for the permissible concentration of impurities. These components might be harmful to the quality of the products, impair the production process and be hazardous to the environment. The goal of the present work is the development of a method for the determination of fluorine in copper concentrate using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis. The molecular absorption of the diatomic molecule CaF was measured at 606.440nm. The molecule CaF was generated by the addition of 200µg Ca as the molecule-forming reagent; the optimized pyrolysis and vaporization temperatures were 900°C and 2400°C, respectively. The characteristic mass and limit of detection were 0.5ng and 3ng, respectively. Calibration curves were established using aqueous standard solutions containing the major components Cu, Fe, S and the minor component Ag in optimized concentrations. The accuracy of the method was verified using certified reference materials. Fourteen copper concentrate samples from Chile and Australia were analyzed to confirm the applicability of the method to real samples; the concentration of fluorine ranged from 34 to 5676mgkg -1 . The samples were also analyzed independently at Analytik Jena by different operators, using the same equipment, but different target molecules, InF and GaF, and different operating conditions; but with a few exceptions, the results agreed quite well. The results obtained at Analytik Jena using the GaF molecule and our results obtained with CaF, with one exception, were also in agreement with the values informed by the supplier of the samples, which were obtained using ion selective electrode potentiometry after alkaline fusion. A comparison will

  14. 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.

  15. Hollow fiber liquid phase microextraction combined with graphite furnace atomic absorption spectrometry for the determination of methylmercury in human hair and sludge samples

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Hongmei [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn; Chen Beibei; Zu Wanqing [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2008-07-15

    Two methods, based on hollow fiber liquid-liquid-liquid (three phase) microextraction (HF-LLLME) and hollow fiber liquid phase (two phase) microextraction (HF-LPME), have been developed and critically compared for the determination of methylmercury content in human hair and sludge by graphite furnace atomic absorption spectrometry (GFAAS). In HF-LPME, methylmercury was extracted into the organic phase (toluene) prior to its determination by GFAAS, while inorganic mercury remained as a free species in the sample solution. In HF-LLLME, methylmercury was first extracted into the organic phase (toluene) and then into the acceptor phase (4% thiourea in 1 mol L{sup -1} HCl) prior to its determination by GFAAS, while inorganic mercury remained in the sample solution. The total mercury was determined by inductively coupled plasma-mass spectrometry (ICP-MS), and the levels of inorganic mercury in both HF-LLLME and HF-LPME were obtained by subtracting methylmercury from total mercury. The factors affecting the microextraction of methylmercury, including organic solvent, extraction time, stirring rate and ionic strength, were investigated and the optimal extraction conditions were established for both HF-LLLPME and HF-LPME. With a consumption of 3.0 mL of the sample solution, the enrichment factors were 204 and 55 for HF-LLLPME and HF-LPME, respectively. The limits of detection (LODs) for methylmercury were 0.1 {mu}g L{sup -1} and 0.4 {mu}g L{sup -1} (as Hg) with precisions (RSDs (%), c = 5 {mu}g L{sup -1} (as Hg), n = 5) of 13% and 11% for HF-LLLPME-GFAAS and HF-LPME-GFAAS, respectively. For ICP-MS determination of total mercury, a limit of detection of 39 ng L{sup -} {sup 1} was obtained. Finally, HF-LLLME-GFAAS was applied to the determination of methylmercury content in human hair and sludge, and the recoveries for the spiked samples were in the range of 99-113%. In order to validate the method, HF-LLLME-GFAAS was also applied to the analysis of a certified reference

  16. Determination of chlorine in food samples via the AlCl molecule using high-resolution continuum source molecular absorption spectrometry in a graphite furnace

    Energy Technology Data Exchange (ETDEWEB)

    Fechetia, Miriam; Tognon, Andre Luiz; Veiga, Marcia A.M.S. da, E-mail: mamsveiga@ffclrp.usp.br

    2012-05-15

    Determination of chlorine using the molecular absorption of aluminum mono-chloride (AlCl) at the 261.418 nm wavelength was accomplished by high-resolution continuum source molecular absorption spectrometry using a transversely heated graphite tube furnace with an integrated platform. For the analysis, 10 {mu}L of the sample followed by 10 {mu}L of a solution containing Al-Ag-Sr modifier, (1 g L{sup -1} each), were directly injected onto the platform. A spectral interference due to the use of Al-Ag-Sr as mixed modifier was easily corrected by the least-squares algorithm present in the spectrometer software. The pyrolysis and vaporization temperatures were 500 Degree-Sign C and 2200 Degree-Sign C, respectively. To evaluate the feasibility of a simple procedure for the determination of chlorine in food samples present in our daily lives, two different digestion methods were applied, namely (A) an acid digestion method using HNO{sub 3} only at room temperature, and (B) a digestion method with Ag, HNO{sub 3} and H{sub 2}O{sub 2}, where chlorine is precipitated as a low-solubility salt (AgCl), which is then dissolved with ammonia solution. The experimental results obtained with method B were in good agreement with the certified values and demonstrated that the proposed method is more accurate than method A. This is because the formation of silver chloride prevented analyte losses by volatilization. The limit of detection (LOD, 3{sigma}/s) for Cl in methods A and B was 18 {mu}g g{sup -1} and 9 {mu}g g{sup -1}, respectively, 1.7 and 3.3 times lower compared to published work using inductively coupled plasma optical emission spectrometry, and absolute LODs were 2.4 and 1.2 ng, respectively. - Highlights: Black-Right-Pointing-Pointer HR-CS MAS as technique for Cl determination via AlCl molecule Black-Right-Pointing-Pointer Spectral interference was corrected by the least-squares algorithm. Black-Right-Pointing-Pointer Chorine precipitation as AgCl prevents Cl losses during

  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. Dispersive liquid-liquid microextraction (DLLME combined with graphite furnace atomic absorption spectrometry (GFAAS for determination of trace Cu and Zn in water Samples

    Directory of Open Access Journals (Sweden)

    Ghorbani A.

    2014-07-01

    Full Text Available Dispersive liquid-liquid microextraction (DLLME combined with graphite furnace atomic absorption spectrometry (GFAAS was proposed for the determination of trace amounts of Copper and Zinc ions using 8-hydroxyquinoline (8-HQ as chelating agent. Several factors influencing the microextraction efficiency of Cu and Zn and their subsequent determinations, such as pH, extraction and disperser solvent type and their volume, concentration of the chelating agent and extraction time were studied, and the optimized experimental conditions were established. After extraction, the enrichment factors were 25 and 26 for Cu and Zn, respectively. The detection limits of the method were 0.025 and 0.0033 μg/L for Cu and Zn, and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Cu and Zn were 8.51% and 7.41%, respectively.

  19. 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 ...

  20. Análise direta de sólidos por espectrometria de absorção atômica com atomização em forno de grafite: uma revisão Solid sampling graphite furnace atomic absorption spectrometry: a review

    Directory of Open Access Journals (Sweden)

    Cassiana Seimi Nomura

    2008-01-01

    Full Text Available This is a review of direct analysis using solid sampling graphite furnace atomic absorption spectrometry. Greater emphasis is dedicated to sample preparation, sample homogeneity, calibration and its application to microanalysis and micro-homogeneity studies. The main advantages and some difficulties related to the applicability of this technique are discussed. A literature search on the application of solid sampling graphite furnace atomic absorption spectrometry in trace element determination in many kinds of samples, including biological, clinical, technological and environmental ones, is also presented.

  1. Selenium determination in biological material by atomic absorption spectrophotometry in graphite furnace and using vapor generation

    International Nuclear Information System (INIS)

    Carvalho Vidal, M. de F. de.

    1984-01-01

    The applicability of the atomic absorption spectrophotometry to the determination of selenium in biological material using vapor generation and electrothermal atomization in the graphite furnace was investigated. Instrumental parameters and the analytical conditions of the methods were studied. Decomposition methods for the samples were tested, and the combustion in the Wickbold apparatus was chosen. (author) [pt

  2. 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.

  3. Graphitization of Coke and Its Interaction with Slag in the Hearth of a Blast Furnace

    Science.gov (United States)

    Li, Kejiang; Zhang, Jianliang; Liu, Yanxiang; Barati, Mansoor; Liu, Zhengjian; Zhong, Jianbo; Su, Buxin; Wei, Mengfang; Wang, Guangwei; Yang, Tianjun

    2016-04-01

    Coke reaction behavior in the blast furnace hearth has yet to be fully understood due to limited access to the high temperature zone. The graphitization of coke and its interaction with slag in the hearth of blast furnace were investigated with samples obtained from the center of the deadman of a blast furnace during its overhaul period. All hearth coke samples from fines to lumps were confirmed to be highly graphitized, and the graphitization of coke in the high temperature zone was convinced to start from the coke surface and lead to the formation of coke fines. It will be essential to perform further comprehensive investigations on graphite formation and its evolution in a coke as well as its multi-effect on blast furnace performance. The porous hearth cokes were found to be filled up with final slag. Further research is required about the capability of coke to fill final slag and the attack of final slag on the hearth bottom refractories since this might be a new degradation mechanism of refractories located in the hearth bottom.

  4. Determination of molybdenum, ruthenium, rhodium, and palladium in radioinactive simulated waste of the nuclear fuel cycle by solid sampling graphite furnace atomic absorption spectrometry (GFAAS)

    International Nuclear Information System (INIS)

    Schmiedel, G.; Mainka, E.; Ache, H.J.

    1989-01-01

    In relation with insoluble particles in the nuclear fuel cycle waste, the solid sampling GFAAS was used to determine molybdenum, ruthenium, rhodium, and palladium in such waste. Two methods for the direct determination of these elements are described. The samples must be handled in glove boxes or moreover in hot cells with a robot. The determination of the elements by the cup-in-tube technique needs a very sensitive balance (microbalance) for weighing in μg-range and the handling of this method is not practical in glove boxes and hot cells. An alternative technique of solid sampling GFAAS, which can be used without great problems in glove boxes and hot cells is the slurry technique. In this case two methods have been used. One method uses graphite powder as a diluter, the other is the direct suspension of the sample in a matrix modifier solution. In the case of slurry technique with predilution of the sample with graphite powder, recoveries between 91 and 102% and RSD between 4 and 8% were obtained, whereas in the case of slurry technique with direct suspension of the waste sample recoveries between 91 and 103% and RSD between 14 and 20% for the above mentioned elements were obtained. (orig.)

  5. Graphite Furnace Atomic Absorption Elemental Analysis of Ecstasy Tablets

    OpenAIRE

    French, Holly E.; Went, Michael J.; Gibson, Stuart J.

    2013-01-01

    Abstract: Six metals (Cu, Mg, Ba, Ni, Cr, Pb) were determined in two separate batches of seized ecstasy\\ud tablets by graphite furnace atomic absorption spectroscopy (GFAAS) following digestion with nitric\\ud acid and hydrogen peroxide. Large intra-batch variations were found as expected for tablets produced\\ud in clandestine laboratories. For example, nickel in batch 1 was present in the range 0.47-13.1 ppm and\\ud in batch 2 in the range 0.35-9.06 ppm. Although batch 1 had significantly high...

  6. Determination of technetium by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Kaye, J.H.; Ballou, N.E.

    1978-01-01

    A detection limit of 6 x 10 -11 g has been achieved for measurement of technetium by graphite furnace atomic absorption spectrometry. A commercially available, demountable, hollow cathode lamp was used and both argon and neon were used as fill gases for the lamp. The range of applicability of the method, when the unresolved 2614.23 to 2615.87 A doublet is used for analysis, is from 60 pg to at least 3 ng of technetium per aliquot analyzed. 3 figures, 1 table

  7. Atomization in a graphite furnace with ballast - a method of improvement of reliability of atomic absorption analysis

    International Nuclear Information System (INIS)

    Katskov, D.A.; Grinshtejn, I.L.

    1978-01-01

    For the purpose of improving the reliability with which elements are determined in atomic absorption analysis with atomization in a graphite furnace, a method is proposed based on the use of a furnace with an extra ballast body. A small cylinder of graphite or refractory metal (Ta) placed in the central part of the furnace, is used as ballast. When in poor heat contact with the wall the ballast is heated by ray emission at a somewhat slower rate than the furnace. It is shown that the kinetics of evaporation of the substance being analysed in the ballast furnace is determined by the rate of change of temperature of the ballast body. As a result of the lag in evaporation, vapour from the analysed substance reaches a zone of a much higher temperature than with evaporation in the usual type furnace, leading to an increase in the degree of atomization. Theoretical analysis establishes the temperature of the ballast, and conditions for the determination of elements (Cd) are optimized. The experiments conducted indicate a considerable decrease in the effect of the composition of the sample on the results of the analysis and a lower molecular interference in the ballast furnace. With high evaporation lag the vapours of the sample reach the zone of practically constant temperature, thus making it possible to use the integral method of absorption registration with absolute accuracy. With fractionated distillation of volatile components of the sample, fractionation is considerably more accurate in a ballast furnace than in the usual type furnace

  8. 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.

  9. Poly(1-vinylimidazole) functionalized magnetic ion imprinted polymer for fast and selective extraction of trace gold in geological, environmental and biological samples followed by graphite furnace atomic absorption spectrometry detection

    Science.gov (United States)

    Zhao, Bingshan; He, Man; Chen, Beibei; Xu, Hongrun; Hu, Bin

    2018-05-01

    In this study, poly(1-vinylimidazole) functionalized gold ion imprinted polymer coated magnetic nanoparticles (MNPs@PVIM-Au-IIP) were prepared and characterized. The adsorption behaviors of the prepared MNPs@PVIM-Au-IIP toward gold ions (Au(III)) were studied, it was found that MNPs@PVIM-Au-IIP has good selectivity, high adsorption capacity (185.4 mg g-1) and fast adsorption kinetic for Au(III). Based on it, a new method of ion imprinted magnetic solid phase extraction (II-MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the analysis of trace Au(III) in real samples with complicated matrix. Factors affecting MSPE including sample pH, desorption reagent, elution concentration and volume, elution time, sample volume and adsorption time were optimized. With high enrichment factor of 100-fold, the detection limit of the proposed method is 7.9 ng L-1 for Au(III) with the relative standard deviation of 7.4% (c = 50 ng L-1, n = 7). In order to validate the accuracy of the proposed method, the Certified Reference Material of GBW07293 geological sample (platinpalladium ore) was analyzed, and the determined value was in good agreement with the certified value. The proposed II-MSPE-GFAAS method is simple, fast, selective, sensitive and has been successfully applied in the determination of trace Au in ore, sediment, environmental water and human urine samples with satisfactory results.

  10. 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).

  11. Air-assisted Liquid Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry for Preconcentration and Determination of Trace Amount of Co(II and Ni(II Ions in Water Samples

    Directory of Open Access Journals (Sweden)

    Saeed Mohammad Sorouraddin

    2017-12-01

    Full Text Available A simple, rapid and efficient method has been developed for the extraction, preconcentration and determination of cobalt (II and nickel (II ions in water samples by air-assisted liquid-liquid microextraction (AALLME coupled with graphite furnace atomic absorption spectrometry (GFAAS. In the proposed method, much less volume of an organic solvent was used as the extraction solvent in the absence of disperser solvent. Fine organic droplets were formed by sucking and injecting of the mixture of aqueous sample solution and extraction solvent with a syringe for several times in a conical test tube. After extraction, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by GFAAS. Several variables that could affect the extraction efficiency were investigated and optimized. Calibration graphs were linear in the range of 6.5-100 ng L-1. Detection limits for Co and Ni were 2.3 ng L-1 and 3 ng L-1, respectively. The accuracy of the developed procedure was checked by analyzing NRCC-SLRS4 Riverine water as a certified reference material. Finally, the proposed method has been successfully applied for the determination of cobalt (II and nickel (II ions in tap, surface and river water samples.

  12. 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

    2018-06-01

    Persistent sample circulation microextraction (PSCME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was developed as a high pre-concentration technique for the determination of heavy metals in fish species. In this method, a few microliters of organic solvent (40.0 µL carbon tetrachloride) was transferred to the bottom of a conical sample cup. Then 10.0 mL of aqueous solution was transformed to fine droplets while passing through the 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 optimal 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 detection (LODs) were in the range of 0.01-0.05 µg kg -1 . Repeatability (intra-day) and reproducibility (inter-day) for 0.50 µg L -1 Hg and 0.10 µg L -1 Cd and Pb were in the range of 3.1-4.2% (n = 7) and 4.3-6.1% (n = 7), respectively. 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. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  13. Graphite furnace atomic absorption elemental analysis of ecstasy tablets.

    Science.gov (United States)

    French, Holly E; Went, Michael J; Gibson, Stuart J

    2013-09-10

    Six metals (copper, magnesium, barium, nickel, chromium and lead) were determined in two separate batches of seized ecstasy tablets by graphite furnace atomic absorption spectroscopy (GFAAS) following digestion with nitric acid and hydrogen peroxide. Large intra-batch variations were found as expected for tablets produced in clandestine laboratories. For example, nickel in batch 1 was present in the range 0.47-13.1 parts per million (ppm) and in batch 2 in the range 0.35-9.06 ppm. Although batch 1 had significantly higher 3,4-methylenedioxy-N-methamphetamine (MDMA) content than batch 2, barium was the only element which discriminated between the two ecstasy seizures (batch 1: 0.19-0.66 ppm, batch 2: 3.77-5.47 ppm). Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

  14. 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.

  15. Determination of vanadium in sea water by graphite furnace atomic absorption spectrometry with a tube coated with pyrolytic graphite

    International Nuclear Information System (INIS)

    Shimizu, Tokuo; Sakai, Kaoru

    1981-01-01

    The trace amount of vanadium in sea water was determined by graphite furnace atomic absorption spectrometry with a tube coated with pyrolytic graphite. To correct the background absorption, a deuterium lamp with a higher-brilliant thermal cathode was used. The sensitivity for vanadium increased 10 -- 20 fold by the use of the tube coated with pyrolytic graphite, and the utility lifetime of the tube was greatly extended. Vanadium(V) - 4-(2-pyridylazo)resorcinol (PAR) complexes were extracted into chloroform as an ion-pair with benzyldimethyltetradecylammonium (Zephiramine) cation alternatively. The sample of sea water, which was made to 0.1 N in sulfuric acid and 0.1% in hydrogen peroxide, was loaded onto the column of Dowex 1-X 4 resin (SO 4 2- -form). Vanadium was then eluted from the resin with 1 N sulfuric acid-0.1% hydrogen peroxide or 1 N hydrochloric acid-0.1% hydrogen peroxide evaporated to dry. After dissolution of the elute in 0.2 N nitric acid, vanadium was extracted. Secondly, the sample of sea water was adjusted to pH 5.0, and loaded onto the column of Chelex-100 resin. Vanadium was eluted from the resin with 2 N ammonia. The above two methods took much time, but the coprecipitation method was not so and recommended for the determination of vanadium in sea water. Vanadium was coprecipitated with iron(III) hydroxide-hydrous titanium(IV) oxide at pH 6.0. The precipitate was digested with nitric acid-hydrogen peroxide. The solution was diluted to 50 ml with water. The resulting solutions were employed to determine the vanadium concentration by the graphite furnace atomic absorption measurement. The trace amounts of vanadium in various kinds of the coastal sea water were determined by the coprecipitation method. (author)

  16. 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.

  17. Graphite electrode DC arc furnace. Innovative technology summary report

    International Nuclear Information System (INIS)

    1999-05-01

    The Graphite Electrode DC Arc Furnace (DC Arc) is a high-temperature thermal process, which has been adapted from a commercial technology, for the treatment of mixed waste. A DC Arc Furnace heats waste to a temperature such that the waste is converted into a molten form that cools into a stable glassy and/or crystalline waste form. Hazardous organics are destroyed through combustion or pyrolysis during the process and the majority of the hazardous metals and radioactive components are incorporated in the molten phase. The DC Arc Furnace chamber temperature is approximately 593--704 C and melt temperatures are as high as 1,500 C. The DC Arc system has an air pollution control system (APCS) to remove particulate and volatiles from the offgas. The advantage of the DC Arc is that it is a single, high-temperature thermal process that minimizes the need for multiple treatment systems and for extensive sorting/segregating of large volumes of waste. The DC Arc has the potential to treat a wide range of wastes, minimize the need for sorting, reduce the final waste volumes, produce a leach resistant waste form, and destroy organic contaminants. Although the DC arc plasma furnace exhibits great promise for treating the types of mixed waste that are commonly present at many DOE sites, several data and technology deficiencies were identified by the Mixed Waste Focus Area (MWFA) regarding this thermal waste processing technique. The technology deficiencies that have been addressed by the current studies include: establishing the partitioning behavior of radionuclides, surrogates, and hazardous metals among the product streams (metal, slag, and offgas) as a function of operating parameters, including melt temperature, plenum atmosphere, organic loading, chloride concentration, and particle size; demonstrating the efficacy of waste product removal systems for slag and metal phases; determining component durability through test runs of extended duration, evaluating the effect of

  18. 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.

  19. Determination of palladium, platinum and rhodium in used automobile catalysts and active pharmaceutical ingredients using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Resano, Martín, E-mail: mresano@unizar.es [Department of Analytical Chemistry, Aragón Institute of Engineering Research (I3A), University of Zaragoza, Pedro Cerbuna 12, 50009 Zaragoza (Spain); Flórez, María del Rosario [Department of Analytical Chemistry, Aragón Institute of Engineering Research (I3A), University of Zaragoza, Pedro Cerbuna 12, 50009 Zaragoza (Spain); Queralt, Ignasi [Institute of Earth Sciences Jaume Almera ICTJA-CSIC, Sole Sabarís s/n, 08028 Barcelona (Spain); Marguí, Eva [Department of Chemistry, Faculty of Sciences, Universitat de Girona, Campus Montilivi s/n, 17071 Girona (Spain)

    2015-03-01

    This work investigates the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for the direct determination of Pd, Pt and Rh in two samples of very different nature. While analysis of active pharmaceutical ingredients is straightforward and it is feasible to minimize matrix effects, to the point that calibration can be carried out against aqueous standard solutions, the analysis of used automobile catalysts is more challenging requiring the addition of a chemical modifier (NH{sub 4}F·HF) to help in releasing the analytes, a more vigorous temperature program and the use of a solid standard (CRM ERM®-EB504) for calibration. However, in both cases it was possible to obtain accurate results and precision values typically better than 10% RSD in a fast and simple way, while only two determinations are needed for the three analytes, since Pt and Rh can be simultaneously monitored in both types of samples. Overall, the methods proposed seem suited for the determination of these analytes in such types of samples, offering a greener and faster alternative that circumvents the traditional problems associated with sample digestion, requiring a small amount of sample only (0.05 mg per replicate for catalysts, and a few milligrams for the pharmaceuticals) and providing sufficient sensitivity to easily comply with regulations. The LODs achieved were 6.5 μg g{sup −1} (Pd), 8.3 μg g{sup −1} (Pt) and 9.3 μg g{sup −1} (Rh) for catalysts, which decreased to 0.08 μg g{sup −1} (Pd), 0.15 μg g{sup −1} (Pt) and 0.10 μg g{sup −1} (Rh) for pharmaceuticals. - Highlights: • Solid sampling HR CS GFAAS permits the fast and direct determination of Pd, Pt and Rh. • 2 determinations suffice for the 3 elements (2 of them can be measured simultaneously). • Samples as different as car catalysts and pharmaceuticals can be accurately analyzed. • Aqueous standards (pharmaceuticals) or a solid CRM (catalysts) is used for calibration.

  20. Development of mixed-waste analysis capability for graphite furnace atomic absorption spectrophotometry

    International Nuclear Information System (INIS)

    Bass, D.A.; TenKate, L.B.; Wroblewski, A.

    1995-03-01

    Graphite furnace atomic absorption spectrophotometer (GFAAS) are typically configured with ventilation to capture potentially toxic and corrosive gases emitted from the vaporization of sample aliquots. When radioactive elements are present, additional concerns (such as meeting safety guidelines and ALARA principles) must be addressed. This report describes a modification to a GFAAS that provides additional containment of vaporized sample aliquots. The modification was found to increase containment by a factor of 80, given expected operating conditions. The use of the modification allows more mixed-waste samples to be analyzed, permits higher levels of radioactive samples to be analyzed, or exposes the analyst to less airborne radioactivity. The containment apparatus was attached to a Perkin-Elmer Zeeman 5000 spectrophotometer for analysis of mixed-waste samples; however, it could also be used on other systems and in other applications where greater containment of vaporized material is desired

  1. Determination of trace amounts of cadmium in zirconium and its alloys by graphite furnace AAS

    International Nuclear Information System (INIS)

    Takashima, Kyoichiro; Toida, Yukio

    1994-01-01

    Trace amount of cadmium in zirconium and its alloys was determined by graphite furnace atomic absorption spectrometry (GF-AAS) after ion exchange separation. A 2g chip sample was decomposed with 20ml of hydrofluoric acid (1+9) and a few drops of nitric acid. A trace amount of cadmium was separated from zirconium by strongly acidic cation-exchange resin (MCI GEL CK 08P) using 50ml of hydrochloric acid as an eluent. The solution was gently evaporated to dryness on an electric hot plate heater and under an infrared lamp. The residue was dissolved in 1ml of nitric acid (1+14) and diluted to 10ml in a volumetric glass flask with distilled water. Ten microliters of this solution was injected into a graphite furnace and then atomized at 2200degC for 4s in argon at a flow rate of 3.0l/min. Acids used in the analytical procedure were purified by azeotropic distillation and cation-exchange resin. The limit of determination (3σ BK ) for cadmium was 0.5ngCd/g and the relative standard deviation (RSD) at 1ngCd/g level was less than 20% for the GF-AAS. The accuracy of this technique was confirmed by NIST SRM 1643b (trace elements in water). (author)

  2. 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.

  3. The method of the atomic-absorption analysis in a graphite furnace with the metallic collector-ballast

    International Nuclear Information System (INIS)

    Katskov, D.A.; Vasil'eva, L.A.; Grinshtejn, I.L.; Savel'eva, G.O.

    1987-01-01

    New method of atomic-absorption analysis in a graphite furnace with the metallic collector-ballast (tungsten were) is suggested. It enables to widen the number of analyzed objects of liquid products wetting readily graphite and metals. It is shown that application of metallic collector-ballast enables to improve sensitivity and reproducibility of analysis, increase the volume of dosed samples as well as to suppress effectively the influence of excess of mineral and organic substrate on results of atomic-absorption analysis of several elements, including Cd, Sr, In, Te

  4. Sub-parts-per-quadrillion-level graphite furnace atomic absorption spectrophotometry based on laser wave mixing.

    Science.gov (United States)

    Mickadeit, Fritz K; Berniolles, Sandrine; Kemp, Helen R; Tong, William G

    2004-03-15

    Nonlinear laser wave mixing in a common graphite furnace atomizer is presented as a zeptomole-level, sub-Doppler, high-resolution atomic absorption spectrophotometric method. A nonplanar three-dimensional wave-mixing optical setup is used to generate the signal beam in its own space. Signal collection is efficient and convenient using a template-based optical alignment. The graphite furnace atomizer offers advantages including fast and convenient introduction of solid, liquid, or gas analytes, clean atomization environment, and minimum background noise. Taking advantage of the unique features of the wave-mixing optical method and those of the graphite furnace atomizer, one can obtain both excellent spectral resolution and detection sensitivity. A preliminary concentration detection limit of 0.07 parts-per-quadrillion and a preliminary mass detection limit of 0.7 ag or 8 zmol are determined for rubidium using a compact laser diode as the excitation source.

  5. [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.

  6. [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.

  7. Graphite electrode DC arc furnace system for treatment of environmentally undesirable solid waste

    International Nuclear Information System (INIS)

    Titus, C.H.

    1993-01-01

    A gas tight DC arc furnace system using graphite electrodes is ideally suited for destruction of organic materials, compaction of metallic materials, and vitrification of inorganic waste materials. A graphite electrode DC arc furnace system which was developed by Electro-Pyrolysis, Inc. has been used to demonstrate that iron basalt soil containing various surrogate nonradioactive materials found on Department of Energy's Atomic Energy Sites and hospital waste can be reduced to a compact, vitrified, solid material which is environmentally acceptable and will pass TCLP leachate tests. A second graphite electrode DC arc furnace system is presently under construction and will be in operation at MIT during the second quarter of 1993. This furnace system is designed for demonstration of waste treatment and stabilization at a rate of 500 pounds per hour and will also be used for development and performance evaluation of diagnostic techniques and equipment for measuring and understanding internal furnace temperature profiles, gas entrained particulate composition, and particulate size distribution in various locations in the furnace during operation

  8. 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...

  9. Titanium Powder Sintering in a Graphite Furnace and Mechanical Properties of Sintered Parts

    Directory of Open Access Journals (Sweden)

    Changzhou Yu

    2017-02-01

    Full Text Available Recent accreditation of titanium powder products for commercial aircraft applications marks a milestone in titanium powder metallurgy. Currently, powder metallurgical titanium production primarily relies on vacuum sintering. This work reported on the feasibility of powder sintering in a non-vacuum furnace and the tensile properties of the as-sintered Ti. Specifically, we investigated atmospheric sintering of commercially pure (C.P. titanium in a graphite furnace backfilled with argon and studied the effects of common contaminants (C, O, N on sintering densification of titanium. It is found that on the surface of the as-sintered titanium, a severely contaminated porous scale was formed and identified as titanium oxycarbonitride. Despite the porous surface, the sintered density in the sample interiors increased with increasing sintering temperature and holding time. Tensile specimens cut from different positions within a large sintered cylinder reveal different tensile properties, strongly dependent on the impurity level mainly carbon and oxygen. Depending on where the specimen is taken from the sintered compact, ultimate tensile strength varied from 300 to 580 MPa. An average tensile elongation of 5% to 7% was observed. Largely depending on the interstitial contents, the fracture modes from typical brittle intergranular fracture to typical ductile fracture.

  10. Surface studies on graphite furnace platforms covered with Pd, Rh and Ir as modifiers in graphite furnace atomic absorption spectrometry of tellurium

    Energy Technology Data Exchange (ETDEWEB)

    Pedro, Juana [Area de Química Analítica, Departamento de Química, Facultad de Ingeniería Química, Universidad Nacional del Litoral, Santiago del Estero 2829 (S3000GL.N), Santa Fe (Argentina); Stripekis, Jorge [Laboratorio de Análisis de Trazas, Departamento de Química Inorgánica, Analítica y Química Física, INQUIMAE, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires, Ciudad Universitaria (1428), Buenos Aires (Argentina); Departamento de Ingeniería Química, Instituto Tecnológico de Buenos Aires, Av. Eduardo Madero 399 (1106), Buenos Aires (Argentina); Bonivardi, Adrian [Area de Química Analítica, Departamento de Química, Facultad de Ingeniería Química, Universidad Nacional del Litoral, Santiago del Estero 2829 (S3000GL.N), Santa Fe (Argentina); Tudino, Mabel, E-mail: tudino@qi.fcen.uba.ar [Laboratorio de Análisis de Trazas, Departamento de Química Inorgánica, Analítica y Química Física, INQUIMAE, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires, Ciudad Universitaria (1428), Buenos Aires (Argentina)

    2015-05-01

    The main objective of this work is the study of correlations between the efficiency of the distribution of the permanent platinum group modifiers Pd, Rh and Ir over the graphite surface with the aim of improving analytical signal of tellurium. Modifier solution was deposited onto the platform and pyrolysed after drying. In the case of Pd, the physical vaporization/deposition technique was also tested. In order to analyze the differences amongst coverings (morphology, topology and distribution), the graphite surfaces were studied with scanning electron microscopy and energy dispersive X-ray microscopy. Micrographs for physical vaporization and pyrolytic deposition of Pd were also analyzed in order to explain the lack of signal obtained for tellurium with the first alternative. Similar micrographs were obtained for pyrolytic deposition of Ir and Rh and then, compared to those of Pd. Ir showed the most homogeneous distribution on the graphite surface and the tallest and sharpest transient. With the aim of improving the analytical signal of tellurium, the correlation between the surface studies and the tellurium transient signal (height, area and shape) is discussed. - Highlights: • Distribution of Rh, Pd and Ir onto graphite furnaces is evaluated by SEM and EDX • Micrographs and spectra showed that surface distribution could influence Te signal. • Ir showed the best signal together with the most homogeneous surface distribution. • Pd-PVD micrographs revealed the absence of graphite and no signal for Te.

  11. 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...... the content of selenium in a selenised yeast check sample. Accuracy was assured using this sample and by recovery experiments. Between-day random error showed a coefficient of variation of 4.2%. Results from the analysis of eight different commercial supplements were in good agreement with declared contents....

  12. Treatment of simulated INEL buried wastes using a graphite electrode DC arc furnace

    International Nuclear Information System (INIS)

    Surma, J.E.; Lawrence, W.E.; Titus, C.H.; Wittle, J.K.; Hamilton, R.A.; Cohn, D.R.; Rhea, D.; Thomas, P.; Woskov, P.P.

    1994-08-01

    A program has been established under the auspices of the Department of Energy (DOE), Office of Technology Development (OTD), to develop the graphite electrode DC arc technology for the application of treating buried heterogenous solid wastes. A three way open-quotes National Laboratory-University-Industryclose quotes partnership was formed to develop this technology in the most timely and cost effective manner. This program is presently testing a newly fabricated pilot-scale DC arc furnace with associated diagnostics at the Plasma Fusion Center at the Massachusetts Institute of Technology. Initial testing in a smaller engineering scale furnace has established the viability of this technology for the treatment of solid heterogeneous wastes. Two diagnostic tools were developed under this program which support the evaluation of the DC arc technology. The diagnostics provide for both spatially resolved temperature measurements within the furnace and real time monitoring of the furnace metal emissions

  13. The determination of magnesium in simulated PWR coolant by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Gatford, C.; Torrance, K.

    1988-06-01

    The determination of magnesium in simulated PWR coolant has been investigated by graphite furnace atomic absorption spectrometry with atomization from a L'vov platform. The presence of boric acid in the coolant suppresses the magnesium absorption to such an extent that removal of the boron is necessary and three variations of a methyl borate volatilization technique for the in situ removal of boron from the sample platform were investigated. This work has shown that dilution of the sample with an equal volume of acidified methanol and volatilization of the methyl borate was adequate for the determination of magnesium in coolant samples containing up to 2000 mg 1 -1 of boron. In simulated coolant samples containing 25 and 4 μg 1 -1 of magnesium, positive biases of about 2 and 0.5 μg 1 -1 were measured and these errors were considered to be due to contamination. The limit of detection in the presence of 100 and 2000 mg 1 -1 boron were 0.14 and 0.93 μg 1 -1 respectively. These performance characteristics suggest the method is completely acceptable for monitoring the chemical purity of PWR coolant and associated waters containing boric acid. If, however, more precise analyses were to be required for research purposes then any significant improvement in the above figures would require increased purity of reagents, clean-room conditions to reduce contamination and a more versatile atomic absorption spectrophotometer. (author)

  14. Formation mechanism of the graphite-rich protective layer in blast furnace hearths

    Science.gov (United States)

    Jiao, Ke-xin; Zhang, Jian-liang; Liu, Zheng-jian; Liu, Feng; Liang, Li-sheng

    2016-01-01

    A long campaign life of blast furnaces is heavily linked to the existence of a protective layer in their hearths. In this work, we conducted dissection studies and investigated damage in blast furnace hearths to estimate the formation mechanism of the protective layer. The results illustrate that a significant amount of graphite phase was trapped within the hearth protective layer. Furthermore, on the basis of the thermodynamic and kinetic calculations of the graphite precipitation process, a precipitation potential index related to the formation of the graphite-rich protective layer was proposed to characterize the formation ability of this layer. We determined that, under normal operating conditions, the precipitation of graphite phase from hot metal was thermodynamically possible. Among elements that exist in hot metal, C, Si, and P favor graphite precipitation, whereas Mn and Cr inhibit this process. Moreover, at the same hot-face temperature, an increase of carbon concentration in hot metal can shorten the precipitation time. Finally, the results suggest that measures such as reducing the hot-face temperature and increasing the degree of carbon saturation in hot metal are critically important to improve the precipitation potential index.

  15. Development of a manufacturing technology of compacted graphite iron castings from a cupola furnace

    Directory of Open Access Journals (Sweden)

    O. Bouska

    2012-01-01

    Full Text Available Compacted graphite iron, also known as vermicular cast iron or semiductile cast iron is a modern material, the production of which is increasing globaly. Recently this material has been very often used in automotive industry. This paper reviews some findigs gained during the development of the manufacturing technology of compacted graphite iron under the conditions in Slévárna Heunisch Brno, Ltd. The new technology assumes usage of cupola furnace for melting and is beeing developed for production of castings weighing up to 300 kilograms poured into bentonite sand moulds.

  16. 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.

  17. Evaluation of the graphite electrode DC arc furnace for the treatment of INEL buried wastes

    International Nuclear Information System (INIS)

    Surma, J.E.; Freeman, C.J.; Powell, T.D.; Cohn, D.R.; Smatlak, D.L.; Thomas, P.; Woskov, P.P.

    1993-06-01

    The past practices of DOE and its predecessor agencies in burying radioactive and hazardous wastes have left DOE with the responsibility of remediating large volumes of buried wastes and contaminated soils. The Buried Waste Integrated Demonstration (BWID), has chosen to evaluate treatment of buried wastes at the Idaho National Engineering Laboratory (INEL). Because of the characteristics of the buried wastes, the potential for using high-temperature thermal treatment technologies is being evaluated. The soil-waste mixture at INEL, when melted or vitrified, produces a glass/ceramic referred to as iron-enriched basalt (IEB). One potential problem with producing the IEB material is the high melting temperature of the waste and soil (1,400-1,600 degrees C). One technology that has demonstrated capabilities to process high melting point materials is the plasma arc heated furnace. A three-party program was initiated and the program involved testing an engineering-scale DC arc furnace to gain preliminary operational and waste processibility information. It also included the design, fabrication, and evaluation of a second-generation, pilot-scale graphite electrode DC arc furnace. Widely ranging simulants of INEL buried waste were prepared and processed in the Mark I furnace. The tests included melting of soils with metals, sludges, combustibles, and simulated drums. Very promising results in terms of waste product quality, volume reduction, heating efficiency, and operational reliability and versatility were obtained. The results indicate that the graphite electrode DC arc technology would be very well suited for treating high melting point wastes such as those found at INEL. The graphite electrode DC arc furnace has been demonstrated to be very simple, yet effective, with excellent prospects for remote or semi-remote operation

  18. High temperature vacuum furnace for the preparation of graphite targets for 14C dating by tandem accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Lowe, D.C.; Bristow, P.; Judd, W.J.

    1985-02-01

    A simple and reliable furnace design capable of producing temperatures of up to 2800 deg. C is presented. The furnace has been specifically designed for the rapid and reliable production of graphite targets for 14 C dating purposes but may be used in a variety of applications requiring high temperatures under vacuum conditions

  19. Determination of cadmium in human urine by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Shimizu, Tokuo; Shijo, Yoshio; Sakai, Kaoru

    1981-01-01

    A trace amount of cadmium in human urine was determined by graphite furnace atomic absorption spectrometry. A urine sample (25 ml) was digested with 5 ml of HNO 3 and 30 ml of H 2 O 2 in a long-neck flask on a hot-plate (200 0 C), then diluted to 50 ml. The standard addition method was carried out before digesting. Ten μl of the resulted solution was injected into a tube treated with tungsten carbide, and the cadmium signal was measured with the ramp mode atomization. Interference induced by organic materials in urine was avoided by HNO 3 -H 2 O 2 digestion. Interference induced by inorganic salts could be reduced by 2-fold dilution and tungsten carbide treatment. The cadmium signal was separated sufficiently from the molecular absorption due to NaCl etc. by the ramp mode atomization. Since the blank level of H 2 O 2 was relatively high, the determination was limited to about 0.1 μg/l. The coefficient of variation was 1.76% at 0.36 μg/l in 24 h human urine (n = 4). The time required was (8 -- 10)h. The precision of this method was higher than those of direct methods, and the reasonable values of urine levels of cadmium were obtained. (author)

  20. Model calculation of the characteristic mass for convective and diffusive vapor transport in graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bencs, László, E-mail: bencs.laszlo@wigner.mta.hu [Institute for Solid State Physics and Optics, Wigner Research Centre for Physics, Hungarian Academy of Sciences, P.O. Box 49, H-1525 Budapest (Hungary); Laczai, Nikoletta [Institute for Solid State Physics and Optics, Wigner Research Centre for Physics, Hungarian Academy of Sciences, P.O. Box 49, H-1525 Budapest (Hungary); Ajtony, Zsolt [Institute of Food Science, University of West Hungary, H-9200 Mosonmagyaróvár, Lucsony utca 15–17 (Hungary)

    2015-07-01

    A combination of former convective–diffusive vapor-transport models is described to extend the calculation scheme for sensitivity (characteristic mass — m{sub 0}) in graphite furnace atomic absorption spectrometry (GFAAS). This approach encompasses the influence of forced convection of the internal furnace gas (mini-flow) combined with concentration diffusion of the analyte atoms on the residence time in a spatially isothermal furnace, i.e., the standard design of the transversely heated graphite atomizer (THGA). A couple of relationships for the diffusional and convectional residence times were studied and compared, including in factors accounting for the effects of the sample/platform dimension and the dosing hole. These model approaches were subsequently applied for the particular cases of Ag, As, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn analytes. For the verification of the accuracy of the calculations, the experimental m{sub 0} values were determined with the application of a standard THGA furnace, operating either under stopped, or mini-flow (50 cm{sup 3} min{sup −1}) of the internal sheath gas during atomization. The theoretical and experimental ratios of m{sub 0}(mini-flow)-to-m{sub 0}(stop-flow) were closely similar for each study analyte. Likewise, the calculated m{sub 0} data gave a fairly good agreement with the corresponding experimental m{sub 0} values for stopped and mini-flow conditions, i.e., it ranged between 0.62 and 1.8 with an average of 1.05 ± 0.27. This indicates the usability of the current model calculations for checking the operation of a given GFAAS instrument and the applied methodology. - Highlights: • A calculation scheme for convective–diffusive vapor loss in GFAAS is described. • Residence time (τ) formulas were compared for sensitivity (m{sub 0}) in a THGA furnace. • Effects of the sample/platform dimension and dosing hole on τ were assessed. • Theoretical m{sub 0} of 18 analytes were

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

    Science.gov (United States)

    Ieggli, C. V. S.; Bohrer, D.; Noremberg, S.; do Nascimento, P. C.; de Carvalho, L. M.; Vieira, S. L.; Reis, R. N.

    2009-06-01

    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 µg L - 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.

  2. 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.

  3. Global analysis of the temperature and flow fields in samples heated in multizone resistance furnaces

    Science.gov (United States)

    Pérez-Grande, I.; Rivas, D.; de Pablo, V.

    The temperature field in samples heated in multizone resistance furnaces will be analyzed, using a global model where the temperature fields in the sample, the furnace and the insulation are coupled; the input thermal data is the electric power supplied to the heaters. The radiation heat exchange between the sample and the furnace is formulated analytically, taking into account specular reflections at the sample; for the solid sample the reflectance is both diffuse and specular, and for the melt it is mostly specular. This behavior is modeled through the exchange view factors, which depend on whether the sample is solid or liquid, and, therefore, they are not known a priori. The effect of this specular behavior in the temperature field will be analyzed, by comparing with the case of diffuse samples. A parameter of great importance is the thermal conductivity of the insulation material; it will be shown that the temperature field depends strongly on it. A careful characterization of the insulation is therefore necessary, here it will be done with the aid of experimental results, which will also serve to validate the model. The heating process in the floating-zone technique in microgravity conditions will be simulated; parameters like the Marangoni number or the temperature gradient at the melt-crystal interface will be estimated. Application to the case of compound samples (graphite-silicon-graphite) will be made; the temperature distribution in the silicon part will be studied, especially the temperature difference between the two graphite rods that hold the silicon, since it drives the thermocapillary flow in the melt. This flow will be studied, after coupling the previous model with the convective effects. The possibility of suppresing this flow by the controlled vibration of the graphite rods will be also analyzed. Numerical results show that the thermocapillary flow can indeed be counterbalanced quite effectively.

  4. 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.

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

    International Nuclear Information System (INIS)

    Wittle, J.K.; Hamilton, R.A.; Trescot, J.

    1995-01-01

    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

  6. Study on graphite samples for nuclear usage

    International Nuclear Information System (INIS)

    Suarez, J.C.M.; Silva Roseira, M. da

    1994-01-01

    Available as short communication only. The graphite, due to its properties (mechanical strength, thermal conductivity, high-temperature stability, machinability etc.) have many industrial applications, and consequently, an important strategic value. In the nuclear area, it has been used as moderator and reflector of neutrons in the fission process of uranium. The graphite can be produced from many types of carbonaceous materials by a variety of process dominated by the manufactures. This is the reason why there are in the world market a lot of graphite types with different physical and mechanical properties. The present investigation studies some physical characteristics of the graphite samples destined to use in a nuclear reactor. (author). 8 refs, 1 fig, 1 tab

  7. The behavior of various chemical forms of nickel in graphite furnace atomic absorption spectrometry under different chemical modification approaches

    International Nuclear Information System (INIS)

    Kowalewska, Zofia

    2012-01-01

    Various organic and inorganic Ni forms were investigated using graphite furnace atomic absorption spectrometry. Experiments without chemical modification showed a wide range of characteristic mass values for Ni (from 6.7 to 29 pg) and the importance of interaction with graphite. With the aim of achieving signal unification of organic Ni forms, different ways of chemical modification were tested. Some rules that govern the behavior of Ni were found and confirmed a significant role of the organic component of the analyte molecule in the analytical process. The application of air as an internal furnace gas in the pyrolysis phase and the Pd modifier injected with the sample solution improved the signal of porphyrins, while the application of iodine and methyltrioctylammonium chloride was required for organic compounds containing oxygen-bound Ni atoms. The Ni signal was strongly diminished when an aqueous solution containing hydrochloric acid was measured with the Pd modifier injected over the sample. Using the developed analytical methods, the range of characteristic mass values for various Ni forms totally dissolved in organic or aqueous solution was 6.5–7.9 pg. - Highlights: ► Some rules that govern behavior of organic Ni forms during GFAAS analysis were found. ► Interaction with graphite can significantly influence evaporation of porphyrins. ► Determination of Ni in form of porphyrins needs Pd organic modifier and air ashing. ► Determination of Ni in O-bound organic compounds needs pretreatment with I2+MTOACl. ► Chemical modification for GFAAS determination of Ni in HCl-containing solution.

  8. Determination of total tin in geological materials by electrothermal atomic-absorption spectrophotometry using a tungsten-impregnated graphite furnace

    Science.gov (United States)

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

    1984-01-01

    An electrothermal atomic-absorption spectrophotometric method is described for the determination of total tin in geological materials, with use of a tungsten-impregnated graphite furnace. The sample is decomposed by fusion with lithium metaborate and the melt is dissolved in 10% hydrochloric acid. Tin is then extracted into trioctylphosphine oxide-methyl isobutyl ketone prior to atomization. Impregnation of the furnace with a sodium tungstate solution increases the sensitivity of the determination and improves the precision of the results. The limits of determination are 0.5-20 ppm of tin in the sample. Higher tin values can be determined by dilution of the extract. Replicate analyses of eighteen geological reference samples with diverse matrices gave relative standard deviations ranging from 2.0 to 10.8% with an average of 4.6%. Average tin values for reference samples were in general agreement with, but more precise than, those reported by others. Apparent recoveries of tin added to various samples ranged from 95 to 111% with an average of 102%. ?? 1984.

  9. Determinação de fósforo em aços por espectrometria de absorção atômica no forno de grafite Determination of phosphorus in steel samples by graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Adilson José Curtius

    1998-06-01

    Full Text Available A method for the determination of phosphorus in steel samples by graphite furnace atomic absorption spectrometry, using the Zeeman effect background correction and the STPF conditions is proposed. The effect of iron (III on the phosphorus signal was studied. It was verified, through the pyrolysis temperature curves, that iron (III is an efficient chemical modifier, thermically stabilizing phosphorus up to 1400ºC. The phosphorus signal increases with the iron (III concentration, but in the range, which corresponds to the usual concentrations of iron in the sample solutions, the increase is small. Phosphorus was determined in three standard reference materials, after its dissolution in a mixture of hydrochloric and perchloric acids in a PTFE bomb. The agreement with the certified concentration values was excellent. Iron (III was added to the reference analytical solutions prepared in the blank of the dissolution, while the sample solutions were measured directly, since they already contained the modifier. The detection limit (k = 2 was 0.0042% of phosphorus in the steel sample.

  10. Dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Zeini Jahromi, Elham; Bidari, Araz; Assadi, Yaghoub; Milani Hosseini, Mohammad Reza; Jamali, Mohammad Reza

    2007-01-01

    Dispersive liquid-liquid microextraction (DLLME) technique was successfully used as a sample preparation method for graphite furnace atomic absorption spectrometry (GF AAS). In this extraction method, 500 μL methanol (disperser solvent) containing 34 μL carbon tetrachloride (extraction solvent) and 0.00010 g ammonium pyrrolidine dithiocarbamate (chelating agent) was rapidly injected by syringe into the water sample containing cadmium ions (interest analyte). Thereby, a cloudy solution formed. The cloudy state resulted from the formation of fine droplets of carbon tetrachloride, which have been dispersed, in bulk aqueous sample. At this stage, cadmium reacts with ammonium pyrrolidine dithiocarbamate, and therefore, hydrophobic complex forms which is extracted into the fine droplets of carbon tetrachloride. After centrifugation (2 min at 5000 rpm), these droplets were sedimented at the bottom of the conical test tube (25 ± 1 μL). Then a 20 μL of sedimented phase containing enriched analyte was determined by GF AAS. Some effective parameters on extraction and complex formation, such as extraction and disperser solvent type and their volume, extraction time, salt effect, pH and concentration of the chelating agent have been optimized. Under the optimum conditions, the enrichment factor 125 was obtained from only 5.00 mL of water sample. The calibration graph was linear in the rage of 2-20 ng L -1 with detection limit of 0.6 ng L -1 . The relative standard deviation (R.S.D.s) for ten replicate measurements of 20 ng L -1 of cadmium was 3.5%. The relative recoveries of cadmium in tap, sea and rivers water samples at spiking level of 5 and 10 ng L -1 are 108, 95, 87 and 98%, respectively. The characteristics of the proposed method have been compared with cloud point extraction (CPE), on-line liquid-liquid extraction, single drop microextraction (SDME), on-line solid phase extraction (SPE) and co-precipitation based on bibliographic data. Therefore, DLLME combined with

  11. 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

  12. 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).

  13. Temperature and flow fields in samples heated in monoellipsoidal mirror furnaces

    Science.gov (United States)

    Rivas, D.; Haya, R.

    The temperature field in samples heated in monoellipsoidal mirror furnaces will be analyzed. The radiation heat exchange between the sample and the mirror is formulated analytically, taking into account multiple reflections at the mirror. It will be shown that the effect of these multiple reflections in the heating process is quite important, and, as a consequence, the effect of the mirror reflectance in the temperature field is quite strong. The conduction-radiation model will be used to simulate the heating process in the floating-zone technique in microgravity conditions; important parameters like the Marangoni number (that drives the thermocapillary flow in the melt), and the temperature gradient at the melt-crystal interface will be estimated. The model will be validated comparing with experimental data. The case of samples mounted in a wall-free configuration (as in the MAXUS-4 programme) will be also considered. Application to the case of compound samples (graphite-silicon-graphite) will be made; the melting of the silicon part and the surface temperature distribution in the melt will be analyzed. Of special interest is the temperature difference between the two graphite rods that hold the silicon part, since it drives the thermocapillary flow in the melt. This thermocapillary flow will be studied, after coupling the previous model with the convective effects. The possibility of counterbalancing this flow by the controlled vibration of the graphite rods will be studied as well. Numerical results show that suppressing the thermocapillary flow can be accomplished quite effectively.

  14. 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.

  15. Furnace

    Energy Technology Data Exchange (ETDEWEB)

    Osintsev, V V; Khidiyatov, A M

    1981-01-01

    The purpose of the invention is to improve the operating efficiency of the furnace device containing prefurnaces connected to the main combustion chamber. For this purpose in the proposed furnace device is equipped with prefurnaces with burners, rectangular vertical chamber of combustion is equipped with central hearth projection. As indicated by studies, the hearth projection of the indicated projections promotes the development of transverse streams which guarantee effective mixing of the combustion products in the upper part of the combustion chamber 3. This reduces the nonuniformity of temperature at the outlet from the latter, decreases the probability of slagging and hot spots on the heating surface.

  16. 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.

  17. Determination of copper and iron in the human aqueous humor by atomic absorption spectrometer with graphite furnace

    International Nuclear Information System (INIS)

    Iqbal, Z.; Mohammad, Z.; Shah, M.T.; Saeed, M.; Imdadullah

    1999-01-01

    The concentration of copper and iron was determined in human aqueous humor using atomic absorption spectrophotometer equipped with graphite furnace. The mean (+- SEM) concentrations of copper (n=16) and iron (n=14) were 0.0234 -+ 0.0045 mu g.ml/sup -1/ and 0.045 -+ 0.0092 mu.ml/sup -1/ respectively. In male and female, the concentrations of copper (p< 0.82) and iron (p<0.38) were not significantly different. (author)

  18. 'Intelligent' triggering methodology for improved detectability of wavelength modulation diode laser absorption spectrometry applied to window-equipped graphite furnaces

    International Nuclear Information System (INIS)

    Gustafsson, Joergen; Axner, Ove

    2003-01-01

    The wavelength modulation-diode laser absorption spectrometry (WM-DLAS) technique experiences a limited detectability when window-equipped sample compartments are used because of multiple reflections between components in the optical system (so-called etalon effects). The problem is particularly severe when the technique is used with a window-equipped graphite furnace (GF) as atomizer since the heating of the furnace induces drifts of the thickness of the windows and thereby also of the background signals. This paper presents a new detection methodology for WM-DLAS applied to a window-equipped GF in which the influence of the background signals from the windows is significantly reduced. The new technique, which is based upon a finding that the WM-DLAS background signals from a window-equipped GF are reproducible over a considerable period of time, consists of a novel 'intelligent' triggering procedure in which the GF is triggered at a user-chosen 'position' in the reproducible drift-cycle of the WM-DLAS background signal. The new methodology makes also use of 'higher-than-normal' detection harmonics, i.e. 4f or 6f, since these previously have shown to have a higher signal-to-background ratio than 2f-detection when the background signals originates from thin etalons. The results show that this new combined background-drift-reducing methodology improves the limit of detection of the WM-DLAS technique used with a window-equipped GF by several orders of magnitude as compared to ordinary 2f-detection, resulting in a limit of detection for a window-equipped GF that is similar to that of an open GF

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

    International Nuclear Information System (INIS)

    Sun Mei; Wu Qianghua

    2010-01-01

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Sun Mei, E-mail: sunmei@ustc.edu.cn [Hefei National Laboratory for Physical Sciences on Microscale, University of Science and Technology of China, No. 96, Jinzhai Road, Hefei 230026 (China); Wu Qianghua [Department of Polymer Science and Engineering, University of Science and Technology of China, Hefei 230026 (China)

    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{sup -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.

  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. Determination of lithium in sodium by vacuum distillation-graphite furnace atomic absorption spectroscopy

    International Nuclear Information System (INIS)

    Xie Chun; Sun Shiping; Jia Yunteng; Wen Ximeng

    1996-12-01

    When sodium is used as a coolant in China Experimental Fast Reactor, the lithium content in sodium has an effect on the nuclear property of reactor. A method has been developed to determine the trace lithium in sodium metal at the level of less than ten parts per million. About 0.4 g sodium is placed into a high-purity tantalum crucible, then it is placed in a stainless-steel still to distill at 360 degree C under vacuum (0.01 Pa). After the sodium has been removed, the residue is dissolved by nitric acid (1:2) and analyzed with Graphite Furnace Atomic Absorption Spectroscopy at 671.0 nm wavelength. The distillation conditions, working conditions of the instrument and interferences from matrix sodium, acid and concomitant elements have been studied. Standard addition experiments are carried out with lithium chloride and lithium nitrate. The percentage recoveries are 96.8% and 97.4% respectively. The relative standard deviation is less than +- 5%. The method has been used to determine lithium content in high pure sodium and industrial grade sodium. (11 refs., 5 figs., 5 tabs.)

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

    Energy Technology Data Exchange (ETDEWEB)

    Calle, Inmaculada de la; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos, E-mail: bendicho@uvigo.es

    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. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

    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. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

  5. 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.

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

    International Nuclear Information System (INIS)

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

    2017-01-01

    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.

  7. Determination of Arsenic in Soil Alkali by Graphite Furnace Atomic Absorption Spectrophotometery Using Modified Corn Silk Fiber as Adsorbent

    International Nuclear Information System (INIS)

    Zhou, X.; Ju, S.; Liu, M.; Zhao, Y.

    2015-01-01

    A safe, rapid, simple and environmentally friendly method based modified corn silk fiber (MC), chemical modified with succinic anhydride (C/sub 4/H/sub 4/O/sub 3/), was developed for the extraction and preconcentration of As(III) in food additives soil alkali sample prior to graphite furnace atomic absorption spectrometry (GFAAS) analysis. The structure and properties of VC (unmodified corn silk fiber) and MC were analyzed and discussed by means of FTIR, SEM and TG, and the effect of adsorbent amount, pH, soil alkali solution concentration, adsorption time and adsorption temperature were carefully optimized. Under the optimum conditions, the relative standard deviations (RSD, n=6) were 1.27-3.05%, the calibration graph was linear in the range of 0-100 meu g/ L and the limits of detection (LOD) was 0.13 meu g/L. The surface of MC became loose and porous which increased the adsorption area. Comparing with VC, carboxy groups were measured in MC and the increase of negative electron group in fiber molecular made its coordination combining ability with As(III) enhanced; In comparison with the removal arsenic rate of VC, MC's significantly increased by 2.86 fold. The recovery rate of soil alkali, treated by VC and MC, reached to 96.85% and 94.32%, and it did not affected the function of soil alkali. (author)

  8. 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...

  9. 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.

  10. Determination of trace concentrations of chlorine in aqueous solutions by high-resolution continuum source graphite furnace molecular absorption spectrometry

    Science.gov (United States)

    Machyňák, Ľubomír; Čacho, František; Němeček, Martin; Beinrohr, Ernest

    2016-11-01

    Trace concentrations of total chlorine were determined by means of molecular absorption of indium mono-chloride (InCl) at 267.217 nm using high-resolution continuum source graphite furnace molecular absorption spectrometry. The effects of chemical modifiers and the amount of In on the sensitivity and accuracy were investigated. The optimum pyrolysis and vaporization temperatures were 600 °C and 1400 °C, respectively. The limit of detection and characteristic mass were found to be 0.10 ng and 0.21 ng, respectively. Potential non-spectral and spectral interferences were tested for various metals and non-metals at concentrations up to 50 mg L- 1 and for phosphoric, sulphuric and nitric acids. No spectral interferences were observed. Significant non-spectral interferences were observed with F, Br, and I at concentrations higher than 1 mg L- 1, 5 mg L- 1 and 25 mg L- 1, respectively, which is probably caused by formation of competitive indium halogen molecules. Higher concentrations of mineral acids depressed the signal owing to the formation of volatile HCl. The calibration curve was linear in the range between 0.3 and 10 ng with a correlation coefficient of R = 0.993. The elaborated method was used for the chlorine determination in various waters and a drug sample.

  11. Characterization of tuyere-level core-drill coke samples from blast furnace operation

    Energy Technology Data Exchange (ETDEWEB)

    S. Dong; N. Paterson; S.G. Kazarian; D.R. Dugwell; R. Kandiyoti [Imperial College London, London (United Kingdom). Department of Chemical Engineering

    2007-12-15

    A suite of tuyere-level coke samples have been withdrawn from a working blast furnace during coal injection, using the core-drilling technique. The samples have been characterized by size exclusion chromatography (SEC), Fourier transform Raman spectroscopy (FT-RS), and X-ray powder diffraction (XRD) spectroscopy. The 1-methyl-2-pyrrolidinone (NMP) extracts of the cokes sampled from the 'bosh', the rear of the 'bird's nest', and the 'dead man' zones were found by SEC to contain heavy soot-like materials (ca. 10{sup 7}-10{sup 8} apparent mass units). In contrast, NMP extracts of cokes taken from the raceway and the front of the 'bird's nest' only contained a small amount of material of relatively lower apparent molecular mass (up to ca. 10{sup 5} u). Since the feed coke contained no materials extractable by the present method, the soot-like materials are thought to have formed during the reactions of volatile matter released from the injectant coal, probably via dehydrogenation and repolymerization of the tars. The Raman spectra of the NMP-extracted core-drilled coke samples showed variations reflecting their temperature histories. Area ratios of D-band to G-band decreased as the exposure temperature increased, while intensity ratios of D to G band and those of 2D to G bands increased with temperature. The graphitic (G), defect (D), and random (R) fractions of the carbon structure of the cokes were also derived from the Raman spectra. The R fractions decreased with increasing temperature, whereas G fractions increased, while the D fractions showed a more complex variation with temperature. These data appear to give clues regarding the graphitization mechanism of tuyere-level cokes in the blast furnace. 41 refs., 9 figs., 6 tabs.

  12. Determination of bromide in aqueous solutions via the TlBr molecule using high-resolution continuum source graphite furnace molecular absorption spectrometry

    Science.gov (United States)

    Cacho, Frantisek; Machynak, Lubomir; Nemecek, Martin; Beinrohr, Ernest

    2018-06-01

    The paper describes the determination of bromide by evaluating the molecular absorption of thallium mono-bromide (TlBr) at the rotational line at 342.9815 nm by making use a high-resolution continuum source graphite furnace atomic absorption spectrometer. The effects of variables such as the wavelength, graphite furnace program, amount of Tl and the use of a modifier were investigated and optimized. Various chemical modifiers have been studied, such as Pd, Mg, Ag and a mixture of Pd/Mg. It was found that best results were obtained by using Ag which prevents losses of bromide during pyrolysis step through precipitation of bromide as AgBr. In this way, a maximum pyrolysis temperature of 400 °C could be used. The optimum molecule forming temperature was found to be 900 °C. Bromide concentrations in various water samples (CRM, bottled drinking water and tap water) were determined. The quantification was made by both linear calibration and standard addition techniques. The results were matched well those of the reference method. The calibration curve was linear in the range between 1 and 1000 ng Br with a correlation coefficient R = 0.999. The limit of detection and characteristic mass of the method were 0.3 ng and 4.4 ng of Br.

  13. Computer programs in BASIC language for graphite furnace atomic absorption using the method of additions. Part 2. Documentation

    International Nuclear Information System (INIS)

    Boyle, W.G. Jr.; Ryan, D.P.

    1979-08-01

    There are four computer programs, written in the BASIC language, used for taking and processing data from an atomic absorption spectrophotometer using the graphite furnace and the method of additions for calibration. The programs chain to each other and are divided into logical sections that have been flow-charted. The chaining sequences, general features, structure, order of subroutines and functions, and the storage of data are discussed. In addition, variables are listed and defined, and a complete listing of each program with a symbol occurrence table is provided

  14. Computer programs in BASIC language for graphite furnace atomic absorption using the method of additions. Part 1. Operating instructions

    International Nuclear Information System (INIS)

    Boyle, W.G. Jr.; Ryan, D.P.

    1979-01-01

    These instructions describe how to use BASIC language programs to process data from atomic absorption spectrophotometers using the graphite furnace and the method of additions calibration technique. The instructions cover loading the programs, responding to computer prompts, choosing among various options for processing the data, performing operations with an automatic sampler, and producing reports. How the programs interact with each other is also explained. Examples of computer/operator dialogue are presented for typical cases. In addition, a concise set of operating instructions is included as an appendix

  15. Preconcentration of trace elements from high-purity thorium and uranium on Chelex-100 and determination by graphite furnace atomic absorption spectrometry with Zeeman-effect background correction

    International Nuclear Information System (INIS)

    Raje, Naina; Kayasth, Satish; Asari, T.P.S.; Gangadharan, S.

    1994-01-01

    Preconcentration of trace impurities from large-sized samples of uranium metal and thorium oxide using a small column of Chelex-100 followed by their determination using graphite furnace atomic absorption spectrometry (GFAAS) is reported. A 0.5-10-g amount of the sample (uranium metal or thorium oxide) was dissolved, complexed with ammonium carbonate and subjected to the ion-exchange procedure. The retained analytes were eluted with 2-4 M nitric acid and brought to a small volume for a final dilution to 10-25 ml for their determination using GFAAS. The validity of the separation procedure and recoveries at μg kg -1 levels was checked by standard addition; the recoveries were >95%

  16. 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.

  17. Graphite furnace analysis of a series of metals (Cu, Mn, Pb, Zn and Cd) in ox kidney

    International Nuclear Information System (INIS)

    Souza, Vivianne L.B. de; Nascimento, Rizia K. do; Paiva, Ana Claudia de; Silva, Josenilda M. da; Melo, Jessica V. de

    2013-01-01

    The aim of this study was to create a methodology for animal tissue analysis, with the use of flame atomic absorption spectrophotometry techniques and graphite furnace analysis to determining metal concentrations in ox kidney. The organ of this animal can be considered a great nutritional food, due to the high protein and micronutrient content beyond the ability to absorb and concentrate important metals such as Zn, Fe, Mn and Se. On the other hand, there is a risk when eating this food owing to the capacity to accumulate toxic metals such as Pb and Cd. In accordance with the laboratory analysis, Zn can be analyzed by flame atomic absorption spectrophotometry, but other metals such as Cu, Mn, Pb and Cd, could only be detected by graphite furnace analysis. The results showed that there is more Zn and Cu than other metals. Such metals follows an order reported by the literature (Zn > Cu > Cd > Pb > Mn). The results showed that kidney is actually a rich source of Zn and Cu. The Cd levels in the ox kidney did not exceed the values which cause toxic effects. The adequacy of the results indicates that the proposed methodology can be used for animal tissue analysis.(author)

  18. Graphite furnace analysis of a series of metals (Cu, Mn, Pb, Zn and Cd) in ox kidney

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Vivianne L.B. de; Nascimento, Rizia K. do; Paiva, Ana Claudia de; Silva, Josenilda M. da, E-mail: vlsouza@cnen.gov.br, E-mail: riziakelia@hotmail.com, E-mail: acpaiva@cnen.gov.br, E-mail: jmnilda@hotmail.com [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil); Melo, Jessica V. de, E-mail: Jessica_clorofila@hotmail.com [Universidade de Pernambuco, Recife, PE (Brazil)

    2013-07-01

    The aim of this study was to create a methodology for animal tissue analysis, with the use of flame atomic absorption spectrophotometry techniques and graphite furnace analysis to determining metal concentrations in ox kidney. The organ of this animal can be considered a great nutritional food, due to the high protein and micronutrient content beyond the ability to absorb and concentrate important metals such as Zn, Fe, Mn and Se. On the other hand, there is a risk when eating this food owing to the capacity to accumulate toxic metals such as Pb and Cd. In accordance with the laboratory analysis, Zn can be analyzed by flame atomic absorption spectrophotometry, but other metals such as Cu, Mn, Pb and Cd, could only be detected by graphite furnace analysis. The results showed that there is more Zn and Cu than other metals. Such metals follows an order reported by the literature (Zn > Cu > Cd > Pb > Mn). The results showed that kidney is actually a rich source of Zn and Cu. The Cd levels in the ox kidney did not exceed the values which cause toxic effects. The adequacy of the results indicates that the proposed methodology can be used for animal tissue analysis.(author)

  19. Cloud point extraction for the determination of lead and cadmium in urine by graphite furnace atomic absorption spectrometry with multivariate optimization using Box-Behnken design

    International Nuclear Information System (INIS)

    Maranhao, Tatiane de A; Martendal, Edmar; Borges, Daniel L.G.; Carasek, Eduardo; Welz, Bernhard; Curtius, Adilson J.

    2007-01-01

    Cloud point extraction (CPE) is proposed as a pre-concentration procedure for the determination of Pb and Cd in undigested urine by graphite furnace atomic absorption spectrometry (GF AAS). Aliquots of 0.5 mL urine were acidified with HCl and the chelating agent ammonium O,O-diethyl dithiophosphate (DDTP) was added along with the non-ionic surfactant Triton X-114 at the optimized concentrations. Phase separation was achieved by heating the mixture to 50 deg. C for 15 min. The surfactant-rich phase was analyzed by GF AAS, employing the optimized pyrolysis temperatures of 900 deg. C for Pb and 800 deg. C for Cd, using a graphite tube with a platform treated with 500 μg Ru as permanent modifier. The reagent concentrations for CPE (HCl, DDTP and Triton X-114) were optimized using a Box-Behnken design. The response surfaces and the optimum values were very similar for aqueous solutions and for the urine samples, demonstrating that aqueous standards submitted to CPE could be used for calibration. Detection limits of 40 and 2 ng L -1 for Pb and Cd, respectively, were obtained along with an enhancement factor of 16 for both analytes. Three control urine samples were analyzed using this approach, and good agreement was obtained at a 95% statistical confidence level between the certified and determined values. Five real samples have also been analyzed before and after spiking with Pb and Cd, resulting in recoveries ranging from 97 to 118%

  20. The radioactivity estimation of 14C and 3H in graphite waste samples of the KRR-2.

    Science.gov (United States)

    Reyoung Kim, Hee

    2013-09-01

    The radioactivity of (14)C and (3)H in graphite samples from the dismantled Korea Research Reactor-2 (the KRR-2) site was analyzed by high-temperature oxidation and liquid scintillation counting, and the graphite waste was suggested to be disposed of as a low-level radioactive waste. The graphite samples were oxidized at a high temperature of 800 °C, and their counting rates were measured by using a liquid scintillation counter (LSC). The combustion ratio of the graphite was about 99% on the sample with a maximum weight of 1g. The recoveries from the combustion furnace were around 100% and 90% in (14)C and (3)H, respectively. The minimum detectable activity was 0.04-0.05 Bq/g for the (14)C and 0.13-0.15 Bq/g for the (3)H at the same background counting time. The activity of (14)C was higher than that of (3)H over all samples with the activity ratios of the (14)C to (3)H, (14)C/(3)H, being between 2.8 and 25. The dose calculation was carried out from its radioactivity analysis results. The dose estimation gave a higher annual dose than the domestic legal limit for a clearance. It was thought that the sampled graphite waste from the dismantled research reactor was not available for reuse or recycling and should be monitored as low-level radioactive waste. Copyright © 2013 Elsevier Ltd. All rights reserved.

  1. 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.

  2. Modified carbon nanotubes as a sorbent for solid-phase extraction of gold, and its determination by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Moghaddam, Firouzeh Hassani; Behzadi, Mansoureh; Naghizadeh, Matin; Taher, Mohammad Ali

    2015-01-01

    A simple, sensitive and accurate method was developed for solid-phase extraction and preconcentration of trace levels of gold in various samples. It is based on the adsorption of gold on modified oxidized multi-walled carbon nanotubes prior to its determination by graphite furnace atomic absorption spectrometry. The type and volume of eluent solution, sample pH value, flow rates of sample and eluent, sorption capacity and breakthrough volume were optimized. Under these conditions, the method showed linearity in the range of 0.2–6.0 ng L −1 with coefficients of determination of >0.99 in the sample. The relative standard deviation for seven replicate determinations of gold (at a level of 0.6 ng L −1 ) is ±3.8 %, the detection limit is 31 pg L −1 (in the initial solution and at an S/N ratio of 3; for n = 8), and the enrichment factor is 200. The sorption capacity of the modified MWCNTs for gold(III) is 4.15 mg g −1 . The procedure was successfully applied to the determination of gold in (spiked) water samples, human hair, human urine and standard reference material with recoveries ranging from 97.0 to 104.2 %. (author)

  3. Feasibility of internal standardization in the direct and simultaneous determination of As, Cu and Pb in sugar-cane spirits by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Caldas, Naise Mary; Ruella Oliveira, Silvana; Anchieta Gomes Neto, Jose

    2009-01-01

    Bismuth and Sb were evaluated as internal standards (IS) to minimize matrix effects on the direct and simultaneous determination of As, Cu, and Pb in cachaca by graphite furnace atomic absorption spectrometry using W-coated platform plus Pd-Mg(NO 3 ) 2 as modifier. For 20 μL injected sample, calibration within the 0.5-10 μg L -1 As, 100-1000 μg L -1 Cu and 0.5-30 μg L -1 Pb intervals were established using the ratios As absorbance to Sb absorbance, Cu absorbance to Bi absorbance and Pb absorbance to Bi absorbance versus analytes concentration, respectively. Typical linear correlations of 0.998, 0.999 and 0.999 were, respectively, obtained. The proposed method was applied for direct determination of As, Cu and Pb in 10 commercial cachaca samples and results were in agreement with those obtained by inductively coupled plasma mass spectrometry at 95% confidence level. The found characteristic masses were 30 pg As, 274 pg Cu and 39 pg Pb. The useful lifetime of the graphite tube was around 760 firings. Recoveries of As, Cu and Pb added to cachaca samples varied, respectively, from 98% to 109%, 97% to 108% and 98% to 104% with internal standards and from 48% to 54%, 53% to 92% and 62% to 97% without internal standards. The limits of detection were 0.13 μg L -1 As, 22 μg L -1 Cu and 0.05 μg L -1 Pb. The relative standard deviations (n = 12) for a spiked sample containing 20 μg L -1 As, Pb and 500 μg L -1 Cu were 1.6%, 1.0%, and 1.8% with IS and 4.3%, 5.2%, and 5.5% without IS

  4. Speciation and determination of ultra trace amounts of chromium by solidified floating organic drop microextraction (SFODME) and graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Moghadam, Masoud Rohani [Department of Chemistry, Faculty of Science, Yazd University, Yazd 89195-741 (Iran, Islamic Republic of); Dadfarnia, Shayessteh, E-mail: sdadfarnia@yazduni.ac.ir [Department of Chemistry, Faculty of Science, Yazd University, Yazd 89195-741 (Iran, Islamic Republic of); Haji Shabani, Ali Mohammad [Department of Chemistry, Faculty of Science, Yazd University, Yazd 89195-741 (Iran, Islamic Republic of)

    2011-02-15

    Solidified floating organic drop microextraction (SFODME) method in combination with graphite furnace atomic absorption spectrometry (GFAAS) has been used for the determination of chromium species in water and urine samples. 1-undecanol containing 2-thenoyltrifluoroacetone (TTA) was used as a selective chelating agent for the extraction of Cr(III). The total Cr was determined after the reduction of Cr(VI) to Cr(III) with hydroxylamine. The concentration of Cr(VI) was determined from the difference between the concentration of total chromium and the Cr(III). Several variables such as the sample pH, concentration of TTA, salt concentration, extraction time and the sample volume were investigated in detail. Under the optimum conditions, the limit of detection of the proposed method was 0.006 {mu}g l{sup -1} for Cr(III) and the relative standard deviation for six replicate determinations at 0.1 {mu}g l{sup -1} Cr(III) was 5.1%. The proposed method was successfully applied for the determination of chromium species in tap water, well water, mineral water, and urine samples.

  5. 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.

  6. 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.

  7. 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.

  8. Multielement preconcentration of trace heavy metals in seawater with an emulsion containing 8-quinolinol for graphite-furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Matsumiya, Hiroaki; Kageyama, Tomohiro; Hiraide, Masataka

    2004-01-01

    A water-in-oil type emulsion containing 8-quinolinol has been used for the concentration of traces of heavy metals from seawater prior to their determinations by graphite-furnace atomic absorption spectrometry. The emulsion used was prepared by dissolving 40 mg of 8-quinolinol and 60 mg of sorbitan monooleate (Span-80) in 3.0 ml of toluene and vigorously mixing with 0.70 ml of aqueous hydrochloric acid solution (1.5 mol l -1 ) by ultrasonic irradiation. The resulting emulsion was gradually injected into 100 ml of sample solution (pH 8.5) and dispersed by stirring as numerous tiny globules. Four heavy metals (Co, Ni, Cu, and Cd) in the sample solution were quantitatively transported through the organic layer into the acidic aqueous droplets encapsulated in the emulsion. After collecting the dispersed emulsion globules, they were demulsified by heating and the heavy metals in the segregated aqueous phase were determined by atomic absorption spectrometry. Owing to the highly efficient concentration (100-fold), these heavy metals at sub-ng ml -1 levels in seawater were determined with satisfactory accuracy and precision, being confirmed with certified reference samples

  9. 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.

  10. CaI and SrI molecules for iodine determination by high-resolution continuum source graphite furnace molecular absorption spectrometry: Greener molecules for practical application.

    Science.gov (United States)

    Zanatta, Melina Borges Teixeira; Nakadi, Flávio Venâncio; da Veiga, Márcia Andreia Mesquita Silva

    2018-03-01

    A new method to determine iodine in drug samples by high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) has been developed. The method measures the molecular absorption of a diatomic molecule, CaI or SrI (less toxic molecule-forming reagents), at 638.904 or 677.692nm, respectively, and uses a mixture containing 5μg of Pd and 0.5μg of Mg as chemical modifier. The method employs pyrolysis temperatures of 1000 and 800°C and vaporization temperatures of 2300 and 2400°C for CaI and SrI, respectively. The optimized amounts of Ca and Sr as molecule-forming reagents are 100 and 150µg, respectively. On the basis of interference studies, even small chlorine concentrations reduce CaI and SrI absorbance significantly. The developed method was used to analyze different commercial drug samples, namely thyroid hormone pills with three different iodine amounts (15.88, 31.77, and 47.66µg) and one liquid drug with 1% m v -1 active iodine in their compositions. The results agreed with the values informed by the manufacturers (95% confidence level) regardless of whether CaI or SrI was determined. Therefore, the developed method is useful for iodine determination on the basis of CaI or SrI molecular absorption. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. [Determination of trace lead and cadmium in transgenic rice by crosslinked carboxymethyl konjac glucomannan microcolumn preconcentration combined with graphite furnace atomic absorption spectrometry].

    Science.gov (United States)

    Liu, Hua-qing; Li, Sheng-qing; Qu, Yang; Chen, Hao

    2012-02-01

    A novel method was developed for the determination of trace lead and cadmium in transgenic brown rice based on separation and preconcentration with a micro column packed with crosslinked carboxymethyl konjac glucomannan (CCMKGM) prior to its determination by graphite furnace atomic absorption spectrometry. Variables affecting the separation and preconcentration of lead and cadmium, such as the acidity of the aqueous solution, sample flow rate and volume, and eluent concentration and volume, were optimized. Under optimized condition, detection limits of the method for the determination of trace lead and cadmium in transgenic brown rice were 0.11 and 0.002 microg x L(-1), respectively. The obtained results of lead and cadmium in the certified reference material (GBW10010, GBS1-1) were in good agreement with the certified values. The recoveries were in the range of 90%-103% and 93%-105% for detection of Pb and Cd in transgenic brown rice and the wild-type brown rice samples respectively. This study could provide technical support for determination of trace Pb and Cd in transgenic rice.

  12. 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

  13. Determination of trace aluminum concentration and homogeneity in biological material TORT-1 by instrumental neutron activation and graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Kratochvil, B.; Motkosky, N.; Duke, M.J.M.; Ng, D.

    1987-01-01

    The biological reference material TORT-1, lobster hepatopancreas, was analyzed for aluminum by instrumental neutron activation analysis (INAA) and graphite furnace atomic absorption spectroscopy (GFAAS). After correction of the INAA results for interferences from 28 Al produced by 31 P(n,α) 28 Al and 28 (n,p) 28 Al reactions, and use of HNO 3 plus HF for sample dissolution for the GFAAS analyses, the methods gave similar results of 43 ± 3 and 42 ± 2 μg/g respectively for 200 to 300-mg test portions. Analysis of six portions from each of six bottles of TORT-1 showed no statistical difference at the 95% confidence level for the between and within bottle variances. Therefore, The material can be considered homogeneous for aluminum if 200- to 300-mg test portions are taken. The variance was greater and the average lower when 30-mg test portions were analyzed for aluminum by GFAAS. The pattern of the results, together with the need for HF in the dissolution procedure, suggests the presence of aluminum-containing microparticulate mineral matter, perhaps silicate material, in the material

  14. Determination of trace aluminum concentration and homogeneity in biological material TORT-1 by instrumental neutron activation and graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kratochvil, B; Motkosky, N; Duke, M J.M.; Ng, D

    1987-05-01

    The biological reference material TORT-1, lobster hepatopancreas, was analyzed for aluminum by instrumental neutron activation analysis (INAA) and graphite furnace atomic absorption spectroscopy (GFAAS). After correction of the INAA results for interferences from /sup 28/Al produced by /sup 31/P(n,..cap alpha..)/sup 28/Al and /sup 28/(n,p)/sup 28/Al reactions, and use of HNO/sub 3/ plus HF for sample dissolution for the GFAAS analyses, the methods gave similar results of 43 +- 3 and 42 +- 2 ..mu..g/g respectively for 200 to 300-mg test portions. Analysis of six portions from each of six bottles of TORT-1 showed no statistical difference at the 95% confidence level for the between and within bottle variances. Therefore, The material can be considered homogeneous for aluminum if 200- to 300-mg test portions are taken. The variance was greater and the average lower when 30-mg test portions were analyzed for aluminum by GFAAS. The pattern of the results, together with the need for HF in the dissolution procedure, suggests the presence of aluminum-containing microparticulate mineral matter, perhaps silicate material, in the material.

  15. Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Bingshan; He, Man; Chen, Beibei; Hu, Bin, E-mail: binhu@whu.edu.cn

    2015-05-01

    Determination of trace Cd in environmental, biological and food samples is of great significance to toxicological research and environmental pollution monitoring. While the direct determination of Cd in real-world samples is difficult due to its low concentration and the complex matrix. Herein, a novel Cd(II)-ion imprinted magnetic mesoporous silica (Cd(II)-II-MMS) was prepared and was employed as a selective magnetic solid-phase extraction (MSPE) material for extraction of trace Cd in real-world samples followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. Under the optimized conditions, the detection limit of the proposed method was 6.1 ng L{sup −1} for Cd with the relative standard deviation (RSD) of 4.0% (c = 50 ng L{sup −1}, n = 7), and the enrichment factor was 50-fold. To validate the proposed method, Certified Reference Materials of GSBZ 50009–88 environmental water, ZK018-1 lyophilized human urine and NIES10-b rice flour were analyzed and the determined values were in a good agreement with the certified values. The proposed method exhibited a robust anti-interference ability due to the good selectivity of Cd(II)-II-MMS toward Cd(II). It was successfully employed for the determination of trace Cd(II) in environmental water, human urine and rice samples with recoveries of 89.3–116%, demonstrating that the proposed method has good application potential in real world samples with complex matrix. - Highlights: • Novel Cd(II)-II-MMS was prepared by surface imprinting combined with a sol–gel process. • Cd(II)-II-MMS has a high selectivity and adsorption capacity for Cd(II). • A sensitive and selective method of Cd(II)-IIMSPE-GFAAS was developed for trace cadmium analysis. • The method can be applied to determine trace Cd in various samples with complicated matrix.

  16. Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection

    International Nuclear Information System (INIS)

    Zhao, Bingshan; He, Man; Chen, Beibei; Hu, Bin

    2015-01-01

    Determination of trace Cd in environmental, biological and food samples is of great significance to toxicological research and environmental pollution monitoring. While the direct determination of Cd in real-world samples is difficult due to its low concentration and the complex matrix. Herein, a novel Cd(II)-ion imprinted magnetic mesoporous silica (Cd(II)-II-MMS) was prepared and was employed as a selective magnetic solid-phase extraction (MSPE) material for extraction of trace Cd in real-world samples followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. Under the optimized conditions, the detection limit of the proposed method was 6.1 ng L −1 for Cd with the relative standard deviation (RSD) of 4.0% (c = 50 ng L −1 , n = 7), and the enrichment factor was 50-fold. To validate the proposed method, Certified Reference Materials of GSBZ 50009–88 environmental water, ZK018-1 lyophilized human urine and NIES10-b rice flour were analyzed and the determined values were in a good agreement with the certified values. The proposed method exhibited a robust anti-interference ability due to the good selectivity of Cd(II)-II-MMS toward Cd(II). It was successfully employed for the determination of trace Cd(II) in environmental water, human urine and rice samples with recoveries of 89.3–116%, demonstrating that the proposed method has good application potential in real world samples with complex matrix. - Highlights: • Novel Cd(II)-II-MMS was prepared by surface imprinting combined with a sol–gel process. • Cd(II)-II-MMS has a high selectivity and adsorption capacity for Cd(II). • A sensitive and selective method of Cd(II)-IIMSPE-GFAAS was developed for trace cadmium analysis. • The method can be applied to determine trace Cd in various samples with complicated matrix

  17. On the possibilities of high-resolution continuum source graphite furnace atomic absorption spectrometry for the simultaneous or sequential monitoring of multiple atomic lines

    International Nuclear Information System (INIS)

    Resano, M.; Rello, L.; Florez, M.; Belarra, M.A.

    2011-01-01

    This paper explores the potential of commercially available high-resolution continuum source graphite furnace atomic absorption spectrometry instrumentation for the simultaneous or sequential monitoring of various atomic lines, in an attempt to highlight the analytical advantages that can be derived from this strategy. In particular, it is demonstrated how i) the monitoring of multiplets may allow for the simple expansion of the linear range, as shown for the measurement of Ni using the triplet located in the vicinity of 234.6 nm; ii) the use of a suitable internal standard may permit improving the precision and help in correcting for matrix-effects, as proved for the monitoring of Ni in different biological samples; iii) direct and multi-element analysis of solid samples may be feasible on some occasions, either by monitoring various atomic lines that are sufficiently close (truly simultaneous monitoring, as demonstrated in the determination of Co, Fe and Ni in NIST 1566a Oyster tissue) or, alternatively, by opting for a selective and sequential atomization of the elements of interest during every single replicate. Determination of Cd and Ni in BCR 679 White cabbage is attempted using both approaches, which permits confirming that both methods can offer very similar and satisfactory results. However, it is important to stress that the second approach provides more flexibility, since analysis is no longer limited to those elements that show very close atomic lines (closer than 0.3 nm in the ultraviolet region) with a sensitivity ratio similar to the concentration ratio of the analytes in the samples investigated.

  18. Determination of tellurium at ultra-trace levels in drinking water by on-line solid phase extraction coupled to graphite furnace atomic absorption spectrometer

    International Nuclear Information System (INIS)

    Pedro, Juana; Stripekis, Jorge; Bonivardi, Adrian; Tudino, Mabel

    2008-01-01

    In this paper, two time-based flow injection (FI) separation pre-concentration systems coupled to graphite furnace atomic absorption spectrometry (GFAAS) for tellurium determination are studied and compared. The first alternative involves the pre-concentration of the analyte onto Dowex 1X8 employed as packaging material of a micro-column inserted in the flow system. The second set-up is based on the co-precipitation of tellurium with La(OH) 3 followed by retention onto XAD resins. Both systems are compared in terms of limit of detection, linear range, RSD%, sample throughput, micro-columns lifetime and aptitude for fully automatic operation. The features of the Dowex system are: 37% efficiency of retention and an enhancement factor of 42 for a pre-concentration time of 180 seconds (sample flow rate = 3 ml min -1 ) with acetic acid elution volumes of 80 μl. The detection limit (3 s) is 7 ng l -1 and the relative standard deviation (n = 7200 ng l -1 ) is 5.8%. The analytical performance of the XAD system is: 72% efficiency of retention and an enhancement factor of 25 for a pre-concentration time of 180 s (sample flow rate = 3 ml min -1 ) with nitric acid elution volumes of 300 μl. The detection limit is 66 ng l -1 and the relative standard deviation (n = 7200 ng l -1 ) is 8.3%. Applications to the determination of tellurium in tap water and the validation of the analytical methodology employing SRM 1643e as certified reference material are shown

  19. Graphite furnace atomic absorption spectrometric determination of vanadium after cloud point extraction in the presence of graphene oxide

    Science.gov (United States)

    López-García, Ignacio; Marín-Hernández, Juan José; Hernández-Córdoba, Manuel

    2018-05-01

    Vanadium (V) and vanadium (IV) in the presence of a small concentration of graphene oxide (0.05 mg mL-1) are quantitatively transferred to the coacervate obtained with Triton X-114 in a cloud point microextraction process. The surfactant-rich phase is directly injected into the graphite atomizer of an atomic absorption spectrometer. Using a 10-mL aliquot sample and 150 μL of a 15% Triton X-114 solution, the enrichment factor for the analyte is 103, which results in a detection limit of 0.02 μg L-1 vanadium. The separation of V(V) and V(IV) using an ion-exchanger allows speciation of the element at low concentrations. Data for seven reference water samples with certified vanadium contents confirm the reliability of the procedure. Several beer samples are also analyzed, those supplied as canned drinks showing low levels of tetravalent vanadium.

  20. Reduction of interferences in graphite furnace atomic absorption spectrometry by multiple linear regression modelling

    Science.gov (United States)

    Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Tiberiade, Christian; Frache, Roberto

    2000-12-01

    The multivariate effects of Na, K, Mg and Ca as nitrates on the electrothermal atomisation of manganese, cadmium and iron were studied by multiple linear regression modelling. Since the models proved to efficiently predict the effects of the considered matrix elements in a wide range of concentrations, they were applied to correct the interferences occurring in the determination of trace elements in seawater after pre-concentration of the analytes. In order to obtain a statistically significant number of samples, a large volume of the certified seawater reference materials CASS-3 and NASS-3 was treated with Chelex-100 resin; then, the chelating resin was separated from the solution, divided into several sub-samples, each of them was eluted with nitric acid and analysed by electrothermal atomic absorption spectrometry (for trace element determinations) and inductively coupled plasma optical emission spectrometry (for matrix element determinations). To minimise any other systematic error besides that due to matrix effects, accuracy of the pre-concentration step and contamination levels of the procedure were checked by inductively coupled plasma mass spectrometric measurements. Analytical results obtained by applying the multiple linear regression models were compared with those obtained with other calibration methods, such as external calibration using acid-based standards, external calibration using matrix-matched standards and the analyte addition technique. Empirical models proved to efficiently reduce interferences occurring in the analysis of real samples, allowing an improvement of accuracy better than for other calibration methods.

  1. 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.

  2. 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.

  3. Cadmium accumulation in the crayfish, Procambarus clarkii, using graphite furnace atomic absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Diaz-Mayans, J.; Hernandez, F.; Medina, J.; Del Ramo, J.; Torreblanca, A.

    1986-11-01

    Lake Albufera and the surrounding rice-field waters are being subject to very heavy loads of sewage and toxic industrial residues (including heavy metals and pesticides) from the many urban and wastewaters in this area. The American red crayfish Procambarus clarkii is native to the Louisiana marshes (USA). In 1978, the crayfish appeared in Lake Albufera near Valencia (Spain), and presently, without adequate sanitary controls, the crayfish is being fished commercially for human consumption. In view of this interest, it is important to have accurate information on concentrations of cadmium in natural waters and cadmium levels of tissues of freshwaters animals used as human food, as well as the accumulation rates of this metal in this animal. In the present study, the authors investigated the accumulation of cadmium in several tissues of the red crayfish, P clarkii (Girard) from Lake Albufera following cadmium exposure. Determinations of cadmium were made by flameless atomic absorption spectroscopy and the standard additions method. Digestion of samples was made by wet ashing in open flasks with concentrated HNO/sub 3/ at 80-90/sup 0/C.

  4. Simultaneous determination of cadmium, iron and tin in canned foods using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Leao, Danilo J; Junior, Mario M S; Brandao, Geovani C; Ferreira, Sergio L C

    2016-06-01

    A method was established to simultaneously determine cadmium, iron and tin in canned-food samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). The quantification step has been performed using the primary line (228.802nm) for cadmium and the adjacent secondary lines (228.725nm and 228.668nm) for iron and tin, respectively. The selected chemical modifier was an acid solution that contained a mixture of 0.1% (w/v) Pd and 0.05% (w/v) Mg. The absorbance signals were measured based on the peak area using 3 pixels for cadmium and 5 pixels for iron and tin. Under these conditions, cadmium, iron and tin have been determined in canned-food samples using the external calibration technique based on aqueous standards, where the limits of quantification were 2.10ngg(-1) for cadmium, 1.95mgkg(-1) for iron and 3.00mgkg(-1) for tin, and the characteristic masses were 1.0pg for cadmium, 0.9ng for iron and 1.1ng for tin. The precision was evaluated using two solutions of each metal ion, and the results, which were expressed as the relative standard deviation (RSD%), were 3.4-6.8%. The method accuracy for cadmium and iron was confirmed by analyzing a certified reference material of apple leaves (NIST 1515), which was supplied by NIST. However, for tin, the accuracy was confirmed by comparing the results of the proposed method and another analytical technique (inductively coupled plasma optical emission spectrometry). The proposed procedure was applied to determine cadmium, iron and tin in canned samples of peeled tomato and sardine. Eleven samples were analyzed, and the analyte concentrations were 3.57-62.9ngg(-1), 2.68-31.48mgkg(-1) and 4.06-122.0mgkg(-1) for cadmium, iron and tin, respectively. In all analyzed samples, the cadmium and tin contents were lower than the permissible maximum levels for these metals in canned foods in the Brazilian legislation. Copyright © 2016. Published by Elsevier B.V.

  5. Analysis of the sensitivity and sample-furnace thermal-lag of a differential thermal analyzer

    International Nuclear Information System (INIS)

    Roura, P.; Farjas, J.

    2005-01-01

    The heat exchange between the horizontal furnace of a differential thermal analyzer (DTA) and the sample is analyzed with the aim of understanding the parameters governing the thermal signal. The resistance due to radiation and conduction through the gas has been calculated and compared to the experimental values of the thermal-lag between the sample and furnace and apparatus sensitivity. The overall evolution of these parameters with the temperature and their relative values are well understood by considering the temperature differences that arise between the sample and holder. Two RC thermal models are used for describing the apparatus performance at different temperature ranges. Finally, the possibility of improving the signal quality through the control of the leak resistances is stressed

  6. Graphite furnace atomic absorption spectrometry with a tantalum boat for the determination of yttrium, samarium, and dysprosium in a mish metal

    International Nuclear Information System (INIS)

    Daidoji, Hidehiro; Tamura, Shohei

    1982-01-01

    The determination of yttrium, samarium, and dysprodium by means of graphite-furnace atomic absorption spectrometry (AAS) was studied by a tantalum boat inserted into a graphite tube atomizer. These elements could not be determined by the use of a commercial graphite tube, In the atomization from a tantalum boat, better analytical sensitivities and negligible memory effects for these rare earths are obtained. The analytical sensitivities of yttrium, samarium, and dysprodium with the tantalum boat were 0.60 ng, 0.86 ng, and 0.17 ng respectively. This method was applied for the determination of yttrium, samarium, and dysprosium in a mish metal. The measurements were performed with slightly acidified solutions (0.01 mol dm 3 HCI or HNO 3 ). The sensitivities and the precisions for these elements decreased with increasing acid concentration. An enhancement in the sensitivities of yttrium and dysprosium upon the addition of a large excess of lanthanum, neodymium, and praseodymium salts were observed. The yttrium, samarium, and dysprosium in a mish metal were determined with both analytical curves of standard solutions containing an excess of lanthanum, cerium, and neodymium ions and of the standard addition. The precisions for this work were in the 3 - 9.3% range. (author)

  7. Study on solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent

    International Nuclear Information System (INIS)

    Yang Guangyu; Fen Weibo; Lei Chun; Xiao Weilie; Sun Handong

    2009-01-01

    A solid phase extraction and graphite furnace atomic absorption spectrometry (GFAAS) for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent was studied. Trace amounts of chromium, nickel, silver, cobalt, copper, cadmium and lead were reacted with 2-(2-quinolinil-azo)-4-methyl-1,3-dihydroxidobenzene (QAMDHB) followed by adsorption onto MCI GEL CHP 20Y solid phase extraction column, and 1.0 mol L -1 HNO 3 was used as eluent. The metal ions in 300 mL solution can be concentrated to 1.0 mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0 g of resin were greater than 95% without interference from alkaline, earth alkaline and some metal ions. When detected with graphite furnace atomic absorption spectrometry, the detection limits in the original samples were 1.4 ng L -1 for Cr(III), 1.0 ng L -1 for Ni(II), 0.85 ng L -1 for Ag(I), 1.2 ng L -1 for Co(II), 1.0 ng L -1 for Cu(II), 1.2 ng L -1 for Cd(II) and 1.3 ng L -1 for Pb(II). The validation of the procedure was performed by the analysis of the certified standard reference materials, and the presented procedure was applied to the determination of analytes in biological, water and soil samples with good results (recoveries range from 89 to 104%, and R.S.D.% lower than 3.2%. The results agreed with the standard value or reference method)

  8. 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.

  9. Second generation laser-heated microfurnace for the preparation of microgram-sized graphite samples

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Bin; Smith, A.M.; Long, S.

    2015-10-15

    We present construction details and test results for two second-generation laser-heated microfurnaces (LHF-II) used to prepare graphite samples for Accelerator Mass Spectrometry (AMS) at ANSTO. Based on systematic studies aimed at optimising the performance of our prototype laser-heated microfurnace (LHF-I) (Smith et al., 2007 [1]; Smith et al., 2010 [2,3]; Yang et al., 2014 [4]), we have designed the LHF-II to have the following features: (i) it has a small reactor volume of 0.25 mL allowing us to completely graphitise carbon dioxide samples containing as little as 2 μg of C, (ii) it can operate over a large pressure range (0–3 bar) and so has the capacity to graphitise CO{sub 2} samples containing up to 100 μg of C; (iii) it is compact, with three valves integrated into the microfurnace body, (iv) it is compatible with our new miniaturised conventional graphitisation furnaces (MCF), also designed for small samples, and shares a common vacuum system. Early tests have shown that the extraneous carbon added during graphitisation in each LHF-II is of the order of 0.05 μg, assuming 100 pMC activity, similar to that of the prototype unit. We use a ‘budget’ fibre packaged array for the diode laser with custom built focusing optics. The use of a new infrared (IR) thermometer with a short focal length has allowed us to decrease the height of the light-proof safety enclosure. These innovations have produced a cheaper and more compact device. As with the LHF-I, feedback control of the catalyst temperature and logging of the reaction parameters is managed by a LabVIEW interface.

  10. 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...

  11. Direct determination of arsenic in petroleum derivatives by graphite furnace atomic absorption spectrometry: A comparison between filter and platform atomizers

    Energy Technology Data Exchange (ETDEWEB)

    Becker, Emilene; Rampazzo, Roger T.; Dessuy, Morgana B. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq - INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Silva, Marcia M. da [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre, RS (Brazil); Welz, Bernhard [Instituto Nacional de Ciencia e Tecnologia do CNPq - INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Katskov, Dmitri A. [Tshwane University of Technology (TUT), Faculty of Science, Chemistry Department, Pretoria 0001 (South Africa)

    2011-05-15

    In the present work a direct method for the determination of arsenic in petroleum derivatives has been developed, comparing the performance of a commercial transversely heated platform atomizer (THPA) with that of a transversely heated filter atomizer (THFA). The THFA results in a reduction of background absorption and an improved sensitivity as has been reported earlier for this atomizer. The mixture of 0.1% (m/v) Pd + 0.03% (m/v) Mg + 0.05% (v/v) Triton X-100 was used as the chemical modifier for both atomizers. The samples (naphtha, gasoline and petroleum condensate) were stabilized in the form of a three-component solution (detergentless microemulsion) with the sample, propan-1-ol and 0.1% (v/v) HNO{sub 3} in a ratio of 3.0:6.4:0.6. The characteristic mass of 13 pg found in the THFA was about a factor of two better than that of 28 pg obtained with the THPA; however, the limits of detection (LOD) and quantification (LOQ) were essentially the same for both atomizers (1.9 and 6.2 {mu}g L{sup -1}, respectively, for THPA, and 1.8 and 5.9 {mu}g L{sup -1}, respectively, for THFA) due to the increased noise observed with the THFA. A possible explanation for that is a partial blockage of the radiation from the hollow cathode lamp by the narrow inner diameter of this tube and the associated loss of radiation energy. Due to the lack of an appropriate certified reference material, recovery tests were carried out with inorganic and organic arsenic standards and the results were between 89% and 111%. The only advantage of the THFA found in this work was a reduction of the total analysis time by about 20% due to the 'hot injection' that could be realized with this furnace. The arsenic concentrations varied from < LOQ to 43.3 {mu}g L{sup -1} in the samples analyzed in this work.

  12. 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...

  13. Investigation of ultraviolet photolysis vapor generation with in-atomizer trapping graphite furnace atomic absorption spectrometry for the determination of mercury

    Energy Technology Data Exchange (ETDEWEB)

    Madden, Jeremy T. [Department of Chemistry, Biochemistry, and Physics, Marist College, 3399 North Road, Poughkeepsie, NY 12601 (United States); Fitzgerald, Neil [Department of Chemistry, Biochemistry, and Physics, Marist College, 3399 North Road, Poughkeepsie, NY 12601 (United States)], E-mail: neil.fitzgerald@marist.edu

    2009-09-15

    Generation of mercury vapor by ultraviolet irradiation of mercury solutions in low molecular weight organic acid solutions prior to measurement by Atomic Absorption Spectrometry is a cheap, simple and green method for determination of trace concentrations of mercury. In this work mercury vapor generated by ultraviolet photolysis was trapped onto a palladium coated graphite furnace significantly improving the detection limit of the method. The system was optimized and a detection limit of 0.12 {mu}g L{sup - 1} (compared to 2.1 {mu}g L{sup - 1} for a previously reported system in the absence of trapping) with a precision of 11% for a 10 {mu}g L{sup - 1} mercury standard (RSD, N = 5)

  14. Study for the determination of samarium, europium,terbium, dysprosium and yttrium in gadolinium oxide matrix by means of atomic absorption spectrophotometry using a graphite furnace

    International Nuclear Information System (INIS)

    Caires, A.C.F.

    1985-01-01

    A study for determination of samarium, europium, terbium, dysprosium and yttrium in a gadolinium oxide matrix by atomic absorption spectrophotometry using a graphite furnace is presented. The best charrring and atomization conditions were estabilished for each element, the most convenient ressonance lines being selected as well. The study was carried out for the mentioned lanthanides both when pure and when in binary mixtures with gadolinium, besides those where all for them were together with gadolinium. The determination limits for pure lanthanides were found to be between 1.3 and 9.6 ng assuming a 20% relative standard deviation as acceptable. The detection limits were in the range 0.51 and 7.5 ng, assuming as positive any answer higher than twofold the standard deviation. (author) [pt

  15. The formation of boron, silicon and calcium containing molecular species in a graphite furnace in Ar/O2 mixtures

    Directory of Open Access Journals (Sweden)

    MILAN MARKICEVIC

    2000-03-01

    Full Text Available The composition of the Ar/O2/C gas system in the presence of traces of either B, Si or Ca was calculated under the assumption of thermal equilibrium in the temperature range 500-5500 K. The mole concentration of oxygen was taken to be 1-4 %. Two sets of calculations were carried out. In the first one the presence of solid phase (graphite was ignored and the calculations were performed for a single-phase (gas system, at variable ratios C/O (0.5, 0.96, 1 and 2. In the second set of calculations the presence of solid carbon (graphite was taken into account and the composition of the gas system in equilibrium with solid carbon, at p = 1 atm, was determined. The results presented show that the equilibrium composition, particularly the concentration of different compounds involving the trace elements , is very sensitive to the amounts, and the ratio of the amounts of oxygen and carbon. Increasing the O/C ratio results in increasing partial pressures of molecular and atomic oxygen, which favours the formation of oxides of the trace elements and moves their atomization temperatures to higher values. On the other hand, increasing the C/O ratio (C/O >>1 favours atomization, but also carbide formation in the lower-temperature region. It was found that, over a relatively wide temperature interval (1000 << T << 3500 K, the composition of the Ar/O2/C/X (X = B, Si, Ca system, with comparable amounts of oxygen and carbon (C/O = 1, does not significantly depend on the presence of the solid phase. The results of calculations enable a reasonable interpretation of numerous experiments carried out on similar systems.

  16. Determination of trace amounts of rare earth elements in samarium, terbium and disprosium oxides by graphite furnace atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Dantas, E.S.K.

    1990-01-01

    A graphite furnace atomic-absorption spectrometry method for the determination of neodymium, europium, terbium, dysprosium and yttrium at trace level in samarium oxide; of samarium, europium, dysprosium, holmium, erbium and yttrium in terbium oxide and of europium, terbium, holmium, erbium and yttrium in dysprosium oxide was established. The best pyrolysis and atomization temperatures were determined for each lanthanide considered. Calibration curves were obtained for the pure elements, for binary mixtures formed by the matrix and each of the lanthanides studied and, finally, for the complex mixtures constituted by the matrix and all the other lanthanide of the group under scrutiny. This study has been carried out to examine the interference of the presence of one lanthanide on the behaviour of the other, since a lack of linearity on the calibration curves has been observed in some cases. Detection and determination limits have been determined as well. The detection limits encountered were within the range 0.002 to 0.3% for different elements. The precision of the method expressed as the relative standard deviation was calculated for each element present in each of the matrices studied. The conclusion arrived at is that the method can be applied for determining the above mentioned lanthanides present in the matrices studied with purity up to 99.50%. (author)

  17. 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

    Energy Technology Data Exchange (ETDEWEB)

    Naeemullah, E-mail: naeemullah433@yahoo.com [Gaziosmanpaşa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Kazi, Tasneem Gul [National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Tuzen, Mustafa [Gaziosmanpaşa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Shah, Faheem; Afridi, Hassan Imran [National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Citak, Demirhan [Gaziosmanpaşa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey)

    2014-02-17

    Graphical abstract: -- Highlights: •A novel and rapid non-dispersive ionic liquid based microextractions. •We used a long narrow glass column to provide more contact area between two media (aqueous and extractive). •APDC using as complexing agent and analyzed by GFAAS. •Introduced a novel approach that reduced solvent consumption, effort, time. •It was applied for determination of understudy analytes in real water sample. -- Abstract: 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 [C{sub 4}mim][PF{sub 6}]. 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{sup −1} and 150, respectively. Reliability of the model method was checked by relative standard deviation (%RSD), which was found to be < 5%. Validity and accuracy of the developed method was checked by analysis of certified reference 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)

  18. Biosorption of aluminum on Pseudomonas aeruginosa loaded on Chromosorb 106 prior to its graphite furnace atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    Tuzen, Mustafa; Soylak, Mustafa

    2008-01-01

    A biosorption procedure for separation-enrichment of aluminum in environmental samples has been presented in this work. Pseudomonas aeruginosa loaded on Chromosorb 106 has been used as biosorbent for that purpose. P. aeruginosa is a gram-negative, aerobic rod. The influences of pH of the aqueous solution, eluent type, eluent volume, sample volume, etc. were examined on the quantitative recovery of aluminum in P. aeruginosa loaded on Chromosorb 106. The effects of concomitant ions on the recoveries of aluminum were also investigated. The detection limit based on 3 sigma for aluminum is 30 ng L -1 . Three certified reference materials (LGC 6010 Hard Drinking Water, NIST-SRM 1568a Rice Flour and NRCC-DORM-2 Dogfish Muscle) were analyzed for the validation of the presented procedure. The proposed procedure was applied to the determination of aluminum in environmental samples including natural water and food samples. The concentration of aluminum in real samples was found at ppb level

  19. Lead determinations in human bone by particle induced x-ray emission (PIXE) and graphite furnace atomic absorption spectrometry (GFAAS)

    Energy Technology Data Exchange (ETDEWEB)

    Deibel, M A; Savage, J M; Robertson, J D; Ehmann, W D [Kentucky Univ., Lexington, KY (United States). Dept. of Chemistry; Markesbery, W R [Kentucky Univ., Lexington, KY (United States)

    1995-08-01

    Chronic lead (Pb) intoxication has been linked to Alzheimer`s disease (AD). Lead, like many heavy elements, tends to accumulate in bone. Pixe is a powerful analytical tool which permits the determination of Pb at the {mu}g/g level without requiring sample digestion. GFAAS is one of the most sensitive methods for the determination of Pb and is capable of determining ng/g levels is solution. For bone analyses by GFAAS, sample dissolution and a matrix modifier are required. Rib bone samples were analyzed for Pb by PIXE and GFAAS. IAEA Animal Bone (H-5) was used as a secondary standard for Pb with both methods to ensure accuracy. The range of Pb concentrations in human rib bone was 1.4-11.5 {mu}/g for the trabecular surface by PIXE, 1.3-45 {mu}g/g for the cortical surface by PIXE, and 1.54-11.75 {mu}g/g for whole bone by GFAAS. No significant difference p.<0.05 was found for AD versus control for either surface or for whole bone. (author). 17 refs., 2 figs., 3 tabs.

  20. Biosorption of platinum and palladium for their separation/preconcentration prior to graphite furnace atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Godlewska-Zylkiewicz, Beata E-mail: bgodlew@uwb.edu.pl

    2003-08-15

    Inexpensive baker's yeast Saccharomyces cerevisiae and green algae Chlorella vulgaris, either free or immobilized on silica gel have been shown to selectively accumulate platinum and palladium from water samples in acidic medium (pH 1.6-1.8). Optimization of conditions of metals biosorption (sample pH, algae and yeast masses, adsorption time, temperature) was performed in batch mode. The procedure of matrix separation based on biosorption of platinum and palladium on algae C. vulgaris covalently immobilized on silica gel in flow mode was developed. The use of algae in flow procedure offers several advantages compared with its use in the batch mode. The procedure shows better reproducibility (<2%), improved efficiency of platinum retention on the column (93.3{+-}1.6%), is less laborious and less time consuming. The best recovery of biosorbed metals from column (87.7{+-}3.3% for platinum and 96.8{+-}1.1 for palladium) was obtained with solution of 0.3 mol l{sup -1} thiourea in 1 mol l{sup -1} hydrochloric acid. The influence of thiourea on analytical signals of examined metals during GFAAS determination is discussed. The procedure has been applied for separation of noble metals from tap and waste water samples spiked with platinum and palladium.

  1. Lead determinations in human bone by particle induced x-ray emission (PIXE) and graphite furnace atomic absorption spectrometry (GFAAS)

    International Nuclear Information System (INIS)

    Deibel, M.A.; Savage, J.M.; Robertson, J.D.; Ehmann, W.D.

    1995-01-01

    Chronic lead (Pb) intoxication has been linked to Alzheimer's disease (AD). Lead, like many heavy elements, tends to accumulate in bone. Pixe is a powerful analytical tool which permits the determination of Pb at the μg/g level without requiring sample digestion. GFAAS is one of the most sensitive methods for the determination of Pb and is capable of determining ng/g levels is solution. For bone analyses by GFAAS, sample dissolution and a matrix modifier are required. Rib bone samples were analyzed for Pb by PIXE and GFAAS. IAEA Animal Bone (H-5) was used as a secondary standard for Pb with both methods to ensure accuracy. The range of Pb concentrations in human rib bone was 1.4-11.5 μ/g for the trabecular surface by PIXE, 1.3-45 μg/g for the cortical surface by PIXE, and 1.54-11.75 μg/g for whole bone by GFAAS. No significant difference (p.<0.05 was found for AD versus control for either surface or for whole bone. (author). 17 refs., 2 figs., 3 tabs

  2. 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

  3. 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.

  4. 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%).

  5. Spectrometer system using a modular echelle spectrograph and a laser-driven continuum source for simultaneous multi-element determination by graphite furnace absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Geisler, Sebastian; Okruss, Michael; Becker-Ross, Helmut; Huang, Mao Dong, E-mail: huang@isas.de; Esser, Norbert; Florek, Stefan

    2015-05-01

    A multi-element absorption spectrometer system has been developed based on a laser-driven xenon continuum source and a modular simultaneous echelle spectrograph (MOSES), which is characterized by a minimized number of optical components resulting in high optical throughput, high transmittance and high image quality. The main feature of the new optical design is the multifunction usage of a Littrow prism, which is attached on a rotation stage. It operates as an order-sorter for the echelle grating in a double-pass mode, as a fine positioning device moving the echelle spectrum on the detector, and as a forwarder to address different optical components, e.g., echelle gratings, in the setup. Using different prisms, which are mounted back to back on the rotation stage, a multitude of different spectroscopic modes like broad-range panorama observations, specific UV–VIS and NIR studies or high resolution zoom investigations of variable spectral channels can be realized. In the UV panorama mode applied in this work, MOSES has simultaneously detectable wavelength coverage from 193 nm to 390 nm with a spectral resolution λ/Δλ of 55,000 (3-pixel criterion). In the zoom mode the latter can be further increased by a factor of about two for a selectable section of the full wavelength range. The applicability and the analytical performance of the system were tested by simultaneous element determination in a graphite furnace, using eight different elements. Compared to an instrument operating in the optimized single line mode, the achieved analytical sensitivity using the panorama mode was typically a factor of two lower. Using the zoom mode for selected elements, comparable sensitivities were obtained. The results confirm the influence of the different spectral resolutions. - Highlights: • Echelle spectrometer with a full frame CCD array detector • High and variable spectral resolution from λ/Δλ of 55,000 to 95,000 • Laser-driven continuum light source

  6. 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

  7. Sample distillation/graphitization system for carbon pool analysis by accelerator mass spectrometry (AMS)

    International Nuclear Information System (INIS)

    Pohlman, J.W.; Knies, D.L.; Grabowski, K.S.; DeTurck, T.M.; Treacy, D.J.; Coffin, R.B.

    2000-01-01

    A facility at the Naval Research Laboratory (NRL), Washington, DC, has been developed to extract, trap, cryogenically distill and graphitize carbon from a suite of organic and inorganic carbon pools for analysis by accelerator mass spectrometry (AMS). The system was developed to investigate carbon pools associated with the formation and stability of methane hydrates. However, since the carbon compounds found in hydrate fields are ubiquitous in aquatic ecosystems, this apparatus is applicable to a number of oceanographic and environmental sample types. Targeted pools are dissolved methane, dissolved organic carbon (DOC), dissolved inorganic carbon (DIC), solid organic matrices (e.g., seston, tissue and sediments), biomarkers and short chained (C 1 -C 5 ) hydrocarbons from methane hydrates. In most instances, the extraction, distillation and graphitization events are continuous within the system, thus, minimizing the possibility of fractionation or contamination during sample processing. A variety of methods are employed to extract carbon compounds and convert them to CO 2 for graphitization. Dissolved methane and DIC from the same sample are sparged and cryogenically separated before the methane is oxidized in a high temperature oxygen stream. DOC is oxidized to CO 2 by 1200 W ultraviolet photo-oxidation lamp, and solids oxidized in sealed, evacuated tubes. Hydrocarbons liberated from the disassociation of gas hydrates are cryogenically separated with a cryogenic temperature control unit, and biomarkers separated and concentrated by preparative capillary gas chromatography (PCGC). With this system, up to 20 samples, standards or blanks can be processed per day

  8. Determinação direta de selênio em água de coco e em leite de coco utilizando espectrometria de absorção atômica com atomização eletrotérmica em forno de grafite Direct determination of selenium in coconut water and coconut milk using graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Poliana C. Aleixo

    2000-06-01

    Full Text Available Selenium is both essential and toxic to man and animals, depending on the concentration and the ingested form. Most fruits and vegetables are poor sources of selenium, but coconut can be a good selenium source. Samples were suspended (1 + 4 v/v in a mixture of tertiary amines soluble in water (10% v/v CFA-C. This simple sample treatment avoided contamination and decreased the analysis time. The standard additions method was adopted for quantification. The action of the autosampler was improved by the presence of the amines mixture in the suspension. A Varian model AA-800 atomic absorption spectrometer equipped with a graphite furnace and a GTA 100 autosampler was used for selenium determination in coconut water and coconut milk. Background correction was performed by means of the Zeeman effect. Pyrolytically coated graphite tubes were employed. Using Pd as chemical modifier, the pyrolysis and the atomization temperatures were set at 1400 and 2200ºC, respectively. For six samples, the selenium concentration in coconut water varied from 6.5 to 21.0 mug L-1 and in coconut milk from 24.2 to 25.1 mug L-1. The accuracy of the proposed method was evaluated by an addition-recovery experiment and all recovered values are in the 99.5-102.3% range. The main advantage of the proposed method is that it can be directly applied without sample decomposition.

  9. Application of Zeeman graphite furnace atomic absorption spectrometry with high-frequency modulation polarization for the direct determination of aluminum, beryllium, cadmium, chromium, mercury, manganese, nickel, lead, and thallium in human blood.

    Science.gov (United States)

    Ivanenko, Natalya B; Solovyev, Nikolay D; Ivanenko, Anatoly A; Ganeev, Alexander A

    2012-10-01

    Determination of aluminum (Al), beryllium (Be), cadmium (Cd), chromium (Cr), mercury (Hg), manganese (Mn), nickel (Ni), lead (Pb), and thallium (Tl) concentrations in human blood using high-frequency modulation polarization Zeeman graphite furnace atomic absorption spectrometry (GFAAS) was performed. No sample digestion was used in the current study. Blood samples were diluted with deionized water or 0.1 % (m/v) Triton X-100 solution for Tl. Dilution factors ranged from 1/5 per volume for Be and Tl to 1/20 per volume for Cd and Pb. For Tl, Cd, and Hg, noble metals (gold, platinum, rhodium, etc.) were applied as surface modifiers. To mitigate chloride interference, 2 % (m/v) solution of NH(4)NO(3) was used as matrix modifier for Tl and Ni assessment. The use of Pd(NO(3))(2) as oxidative modifier was necessary for blood Hg and Tl measurement. Validation of the methods was performed by analyzing two-level reference material Seronorm. The precision of the designed methods as relative SD was between 4 and 12 % (middle of a dynamic range) depending on the element. For additional validation, spiked blood samples were analyzed. Limits of detection (LoDs, 3σ, n = 10) for undiluted blood samples were 2.0 μg L(-1) for Al, 0.08 μg L(-1) for Be, 0.10 μg L(-1) for Cd, 2.2 μg L(-1) for Cr, 7 μg L(-1) for Hg, 0.4 μg L(-1) for Mn, 2.3 μg L(-1) for Ni, 3.4 μg L(-1) for Pb, and 0.5 μg L(-1) for Tl. The LoDs achieved allowed determination of Al, Cd, Cr, Mn, Ni, and Pb at both toxic and background levels. Be, Hg, and Tl could be reliably measured at toxic levels only. The methods developed are used for clinical diagnostics and biological monitoring of work-related exposure.

  10. 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

  11. Investigation of the feasibility to use Zeeman-effect background correction for the graphite furnace determination of phosphorus using high-resolution continuum source atomic absorption spectrometry as a diagnostic tool

    Energy Technology Data Exchange (ETDEWEB)

    Lepri, Fabio G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.b [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Dessuy, Morgana B.; Vale, Maria Goreti R. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre-RS (Brazil); Bohrer, Denise [Departamento de Quimica, Universidade Federal de Santa Maria, 97110-905 Santa Maria, RS (Brazil); Loos-Vollebregt, Margaretha T.C. de [Delft University of Technology, Faculty of Applied Sciences, Analytical Biotechnology, Julianalaan 137, 2628 BL Delft (Netherlands); Department of Analytical Chemistry, Ghent University, Krijgslaan 281 - S12, B-9000 Ghent (Belgium); Mao Donghuang; Becker-Ross, Helmut [ISAS, Institute for Analytical Sciences, Department of Interface Spectroscopy, Albert-Einstein Str. 9, 12489 Berlin (Germany)

    2010-01-15

    The determination of phosphorus by graphite furnace atomic absorption spectrometry at the non-resonance line at 213.6 nm, and the capability of Zeeman-effect background correction (Z-BC) to deal with the fine-structured background absorption due to the PO molecule have been investigated in the presence of selected chemical modifiers. Two line source atomic absorption spectrometers, one with a longitudinally heated and the other with a transversely heated graphite tube atomizer have been used in this study, as well as two prototype high-resolution continuum source atomic absorption spectrometers, one of which had a longitudinally arranged magnet at the furnace. It has been found that Z-BC is capable correcting very well the background caused by the PO molecule, and also that of the NO molecule, which has been encountered when the Pd + Ca mixed modifier was used. Both spectra exhibited some Zeeman splitting, which, however, did not cause any artifacts or correction errors. The practical significance of this study is to confirm that accurate results can be obtained for the determination of phosphorus using Z-BC. The best sensitivity with a characteristic mass of m{sub 0} = 11 ng P has been obtained with the pure Pd modifier, which also caused the lowest background level. The characteristic mass obtained with the mixed Pd+Ca modifier depended on the equipment used and was between m{sub 0} = 9 ng P and m{sub 0} = 15 ng P, and the background signal was higher. The major problem of Z-BC remains the relatively restricted linear working range.

  12. Reviewing the analysis of silicons produced in Iran; design and construction of furnaces to produce lead glass by sintering and analyzing the end products

    International Nuclear Information System (INIS)

    Shariatmadar Qoochan, Sharam.

    1995-01-01

    In this project there was always the need of a furnace and cast; therefore, the work was concentrated on construction the furnace and designing the cast. Many numbers of graphites were prepared and by altering their dimensions it was tried to obtain the best conditions from point of view of material and dimensions. Because in this type of furnace having the proper graphite in fact prepared to work with the furnace, because graphite was the heat transfer to the body and also was the cast of the body. The advantage of using graphite furnaces was the heating up of graphite soon, and there was not the problem of sticking to the cast. The disadvantage was the restriction of dimensions. Therefore, the glass size was also limited. another disadvantage was the temperature range to melt the sample. By varying the glass formulation the melting point of the sample also varied. So that by reducing the lead percentage the melting point increased, and restricted to fabricate glass with low percentage of lead

  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. GEO-MIX-SELF calculations of the elastic properties of a textured graphite sample at different hydrostatic pressures

    International Nuclear Information System (INIS)

    Matthies, Siegfried

    2012-01-01

    The recently developed GEO-MIX-SELF approximation (GMS) is applied to interpret the pressure dependence of the longitudinal ultrasonic wave velocities in a polycrystalline graphite sample that has already been investigated in a wide range of experimental contexts. Graphite single crystals have extremely anisotropic elastic properties, making this sample a challenging test to demonstrate the potential of the GMS method. GMS combines elements of well known self-consistent algorithms and of the geometric mean approximation. It is able to consider mixtures of different polycrystalline phases, each with its own nonspherical grain shape and preferred orientation (texture). Pores and 'cracks', typical for bulk graphite, are modeled as phases with 'empty' grains. The pressure dependence (up to 150 MPa) of the experimental wave velocities can be well explained using the known texture of the sample by fitting the shape parameters and volume fractions of the graphite grains, cracks and spherical pores. The pressure dependence of these parameters describes a reasonable scenario for the closing of the cracks and pores with increasing pressure. (orig.)

  16. Brazing graphite to graphite

    International Nuclear Information System (INIS)

    Peterson, G.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 graphite

  17. Investigating the formation mechanism of soot-like materials present in blast furnace coke samples

    Energy Technology Data Exchange (ETDEWEB)

    S. Dong; P. A' lvarez; N. Paterson; D.R. Dugwell; R. Kandiyoti [Imperial College London, London (United Kingdom). Department of Chemical Engineering

    2008-09-15

    An attempt to gain an understanding of the formation mechanism of these 'soot-like' materials has been made by means of tracing the changes in the molecular-mass distribution and molecular structure of the NMP-extractable materials from an injectant coal as well as its partially gasified chars and its pyrolytic tars. Variations in the SEC chromatograms provide clues about changes in the apparent molecular-mass distributions of these NMP extracts. Results suggest that the build-up of 'soot-like' materials follows from the secondary reactions of tars evolved from the injectant coal. The likely secondary-reaction pathways have been probed by collating structural information on these NMP extracts. The time-resolved 13-16 and 22-25 min elution fractions from the SEC column have been characterized using UV fluorescence (UV F) spectroscopy. Greater concentrations of larger aromatic ring systems are found present in samples formed under conditions appearing more prone for soot formation. The 11-16 min (large apparent molecular mass) effluent from SEC has been examined by Fourier transform infrared (FTIR) spectroscopy and transmission electron microscopy (TEM). Results from FTIR spectroscopy are consistent with the UV F data, showing more significant extents of dehydrogenation under conditions more prone to form soot. Similarly, TEM results show that larger amount of graphene layers exist in samples exposed to more soot-prone conditions. The emerging picture for the formation of 'soot-like' materials involves a well-defined sequence. Tars evolved from the injectant coal undergo secondary dehydrogenation, condensation, and repolymerization reactions, which eventually lead to the formation of the NMP-extractable 'soot-like' materials of large apparent molecular mass. 44 refs., 7 figs., 3 tabs.

  18. Special graphites; Graphites speciaux

    Energy Technology Data Exchange (ETDEWEB)

    Leveque, P [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1964-07-01

    A large fraction of the work undertaken jointly by the Commissariat a l'Energie Atomique (CEA) and the Pechiney Company has been the improvement of the properties of nuclear pile graphite and the opening up of new fields of graphite application. New processes for the manufacture of carbons and special graphites have been developed: forged graphite, pyro-carbons, high density graphite agglomeration of graphite powders by cracking of natural gas, impervious graphites. The physical properties of these products and their reaction with various oxidising gases are described. The first irradiation results are also given. (authors) [French] Ameliorer les proprietes du graphite nucleaire pour empilements et ouvrir de nouveaux domaines d'application au graphite constituent une part importante de l'effort entrepris en commun par le Commissariat a l'Energie Atomique (CEA) et la compagnie PECHINEY. Des procedes nouveaux de fabrication de carbones et graphites speciaux ont ete mis au point: graphite forge, pyrocarbone, graphite de haute densite, agglomeration de poudres de graphite par craquage de gaz naturel, graphites impermeables. Les proprietes physiques de ces produits ainsi que leur reaction avec differents gaz oxydants sont decrites. Les premiers resultats d'irradiation sont aussi donnes. (auteurs)

  19. 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.

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

    Science.gov (United States)

    Kowalewska, Zofia

    2011-07-01

    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 ∆ν = 0 vibrational sequence within the electronic transition X 1∑ + → A 1П, 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 xS 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 -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 -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 sulphur content determined by X-ray fluorescence

  1. 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

  2. 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

  3. Risk management of energy efficiency projects in the industry - sample plant for injecting pulverized coal into the blast furnaces

    OpenAIRE

    Jovanović Filip P.; Berić Ivana M.; Jovanović Petar M.; Jovanović Aca D.

    2016-01-01

    This paper analyses the applicability of well-known risk management methodologies in energy efficiency projects in the industry. The possibilities of application of the selected risk management methodology are demonstrated within the project of the plants for injecting pulverized coal into blast furnaces nos. 1 and 2, implemented by the company US STEEL SERBIA d.o.o. in Smederevo. The aim of the project was to increase energy efficiency through the reductio...

  4. 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

  5. Risk management of energy efficiency projects in the industry - sample plant for injecting pulverized coal into the blast furnaces

    Directory of Open Access Journals (Sweden)

    Jovanović Filip P.

    2016-01-01

    Full Text Available This paper analyses the applicability of well-known risk management methodologies in energy efficiency projects in the industry. The possibilities of application of the selected risk management methodology are demonstrated within the project of the plants for injecting pulverized coal into blast furnaces nos. 1 and 2, implemented by the company US STEEL SERBIA d.o.o. in Smederevo. The aim of the project was to increase energy efficiency through the reduction of the quantity of coke, whose production requires large amounts of energy, reduction of harmful exhaust emission and increase productivity of blast furnaces through the reduction of production costs. The project was complex and had high costs, so that it was necessary to predict risk events and plan responses to identified risks at an early stage of implementation, in the course of the project design, in order to minimise losses and implement the project in accordance with the defined time and cost limitations. [Projekat Ministarstva nauke Republike Srbije, br. 179081: Researching contemporary tendencies of strategic management using specialized management disciplines in function of competitiveness of Serbian economy

  6. [NIR and XRD analysis of drill-hole samples from Zhamuaobao iron-graphite deposit, Inner Mongolia].

    Science.gov (United States)

    Li, Ying-kui; Cao, Jian-jin; Wu, Zheng-quan; Dai, Dong-le; Lin, Zu-xu

    2015-01-01

    The author analyzed the 4202 drill-hole samples from Zhamuaobao iron-graphite deposit by using near infrared spectroscopy(NIR) and X-ray diffraction(XRD) measuring and testing techniques, and then compared and summarized the results of two kinds of testing technology. The results indicate that some difference of the mineral composition exists among different layers, the lithology from upper to deeper is the clay gravel layer of tertiary and quaternary, mudstone, mica quartz schist, quartz actinolite scarn, skarnization marble, iron ore deposits, graphite deposits and mica quartz schist. The petrogenesis in different depth also shows difference, which may indicate the geological characteristic to some extent. The samples had mainly undergone such processes as oxidization, carbonation, chloritization and skarn alteration. The research results can not only improve the geological feature of the mining area, but also have great importance in ore exploration, mining, mineral processing and so on. What's more, as XRD can provide preliminary information about the mineral composition, NIR can make further judgement on the existence of the minerals. The research integrated the advantages of both NIR and XRD measuring and testing techniques, put forward a method with two kinds of modern testing technology combined with each other, which may improve the accuracy of the mineral composition identification. In the meantime, the NIR will be more wildly used in geography on the basis of mineral spectroscopy.

  7. Design and Development of Tilting Rotary Furnace

    Science.gov (United States)

    Sai Varun, V.; Tejesh, P.; Prashanth, B. N.

    2018-02-01

    Casting is the best and effective technique used for manufacturing products. The important accessory for casting is furnace. Furnace is used to melt the metal. A perfect furnace is one that reduces the wastage of material, reduces the cost of manufacturing and there by reduces the cost of production. Of all the present day furnaces there may be wastage of material, and the chances of increasing the time of manufacturing as the is continuous need of tilting of the furnace for every mould and then changing the moulds. Considering these aspects, a simple and least expensive tilting rotary furnace is designed and developed. The Tilting and Rotary Furnace consists of mainly melting chamber and the base. The metal enters the melting chamber through the input door that is provided on the top of the melting chamber. Inside the melting chamber there is a graphite furnace. The metal is melted in the graphite crucible. An insulation of ceramic fibre cloth is provided inside the furnace. The metal is melted using Propane gas. The propane gas is easily available and economic. The gas is burned using a pilot burner. The pilot burner is more efficient that other burners. The pilot burner is lit with a push button igniter. The pilot burner is located at the bottom of the combustion chamber. This enables the uniform heating of the metal inside the crucible. The temperature inside the melting chamber is noted using a temperature sensor. The gas input is cut-off if the temperature is exceeding a specific temperature. After the melting of the metal is done the furnace is tilted and after the mould is filled it is rotated. The external gears are used to controlling the tilting. The results of studies carried out for the design & development of low cost, simple furnace that can be mounted anywhere on the shop floor and this can be very much useful for the education purposes and small scale manufacturing. The furnace can be rotated in 360 degrees and can help in reducing the time taken

  8. Cadmium and lead determination in foods by beam injection flame furnace atomic absorption spectrometry after ultrasound-assisted sample preparation

    International Nuclear Information System (INIS)

    Aleixo, Poliana Carolina; Junior, Dario Santos; Tomazelli, Andrea Cristina; Rufini, Iolanda A.; Berndt, Harald; Krug, Francisco Jose

    2004-01-01

    A simple method for cadmium and lead determination in foods by beam injection flame furnace atomic absorption spectrometry (BIFF-AAS) was proposed. Food slurries were prepared by transferring an exact amount of cryogenic-ground homogenized material (50-100 mg) to centrifuge tubes, followed by addition of 5 ml (up to 2.8 mol l -1 ) nitric acid solution and sonication in an ultrasonic bath during 5-10 min. Thereafter, slurries were diluted with water to 10 ml, centrifuged during 5 min at 5400 rpm and 400 μl aliquot of the supernatant was analyzed by BIFF-AAS. The detection limits based on peak height measurements were 0.03 μg g -1 Cd and 1.6 μg g -1 Pb for 2% (m/v) slurry (200 mg/10 ml). For method validation, the certified reference materials Pig Kidney (BCR 186) and Rice Flour (NIES 10) were used. Quantitative cadmium and lead recoveries were obtained and no statistical differences were found at 95% level by applying the t-test

  9. Molecular absorption spectrometry in flames and furnaces: A review

    Energy Technology Data Exchange (ETDEWEB)

    Butcher, David J., E-mail: butcher@email.wcu.edu

    2013-12-04

    Graphical abstract: -- Highlights: •Theory and analytical considerations for molecular absorption spectrometry (MAS). •Critical review of low resolution MAS. •Critical review of the analytical performance of high-resolution continuum source (HR-CS) flame MAS. •Critical review of the analytical performance of HR-CS graphite furnace MAS. •Current status of HR-CS MAS and its future prospects for elemental analysis. -- Abstract: Molecular absorption spectrometry (MAS), originally developed in the 1970s, is a technique to determine non-metals in flames and graphite furnaces by monitoring the absorbance of diatomic molecules. Early studies employed low resolution instruments designed for line source atomic absorption, which provided a limited choice of analytical wavelengths, insufficient spectral resolution, and spectral interferences. However, the development of high-resolution continuum source atomic absorption spectrometry (HR-CS AAS) instrumentation has allowed the analysis of challenging samples for non-metals as well as some difficult elements to determine by AAS, such as aluminum and phosphorus. In this review, theory and analytical considerations for MAS are discussed. The principles and limitations of low resolution MAS are described, along with its applications. HR-CS AAS instrumentation is reviewed, emphasizing performance characteristics most relevant for MAS. Applications of flame and HR-CS GFMAS are reviewed, highlighting the most significant work to date. The paper concludes with an evaluation of the enhanced analytical capabilities provided by HR-CS MAS.

  10. Special graphites

    International Nuclear Information System (INIS)

    Leveque, P.

    1964-01-01

    A large fraction of the work undertaken jointly by the Commissariat a l'Energie Atomique (CEA) and the Pechiney Company has been the improvement of the properties of nuclear pile graphite and the opening up of new fields of graphite application. New processes for the manufacture of carbons and special graphites have been developed: forged graphite, pyro-carbons, high density graphite agglomeration of graphite powders by cracking of natural gas, impervious graphites. The physical properties of these products and their reaction with various oxidising gases are described. The first irradiation results are also given. (authors) [fr

  11. Atomization mechanisms for barium in furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Styris, D.L.

    1984-01-01

    Atomic absorption spectrometry and mass spectrometry are used simultaneously in order to elucidate atomization mechanisms of barium dichloride in pyrolytic graphite, vitreous carbon, and tantalum furnaces. Gas-phase barium dicarbide is observed to appear concurrently with the free barium. Barium oxide and barium dihydroxide precursors appear with the chlorides. Surface reactions involving species that are absorbed on the various furnaces are postulated to explain the appearances of the species that are observed in the gas phase. 49 references, 4 figures, 1 table

  12. Heat treatment furnace

    Science.gov (United States)

    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.

  13. 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.

    NARCIS (Netherlands)

    Slobodník, J.; Oztekizan, O.; Lingeman, H.; Brinkman, U.A.T.

    1996-01-01

    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

  14. A study of sample mineralization methods for arsenic analysis of blood and urine by hydride generation and graphite furnace atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Sysalová, Jiřina; Spěváčková, V.

    2003-01-01

    Roč. 1, č. 2 (2003), s. 108-120 ISSN 1644-3624 R&D Projects: GA MZd IZ3980 Institutional research plan: CEZ:AV0Z4031919 Keywords : Arsenic * HG AAS * GF AAS Subject RIV: CB - Analytical Chemistry, Separation

  15. Carbon-14 Graphitization Chemistry

    Science.gov (United States)

    Miller, James; Collon, Philippe; Laverne, Jay

    2014-09-01

    Accelerator Mass Spectrometry (AMS) is a process that allows for the analysis of mass of certain materials. It is a powerful process because it results in the ability to separate rare isotopes with very low abundances from a large background, which was previously impossible. Another advantage of AMS is that it only requires very small amounts of material for measurements. An important application of this process is radiocarbon dating because the rare 14C isotopes can be separated from the stable 14N background that is 10 to 13 orders of magnitude larger, and only small amounts of the old and fragile organic samples are necessary for measurement. Our group focuses on this radiocarbon dating through AMS. When performing AMS, the sample needs to be loaded into a cathode at the back of an ion source in order to produce a beam from the material to be analyzed. For carbon samples, the material must first be converted into graphite in order to be loaded into the cathode. My role in the group is to convert the organic substances into graphite. In order to graphitize the samples, a sample is first combusted to form carbon dioxide gas and then purified and reduced into the graphite form. After a couple weeks of research and with the help of various Physics professors, I developed a plan and began to construct the setup necessary to perform the graphitization. Once the apparatus is fully completed, the carbon samples will be graphitized and loaded into the AMS machine for analysis.

  16. On-line preconcentration using a resin functionalized with 3,4-dihydroxybenzoic acid for the determination of trace elements in biological samples by thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Lemos, Valfredo A.; Bezerra, Marcos A.; Amorim, Fabio A.C.

    2008-01-01

    In the present paper, an on-line preconcentration procedure for determination of cadmium, copper and zinc by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is proposed. Amberlite XAD-4 functionalized with 3,4-dihydroxybenzoic acid (XAD4-DHB) packed in a minicolumn was used as sorbent material. The metals were retained on the XAD-DHB resin, from which it could be eluted directly to the thermospray flame furnace system. The detection limits were 28 (Cd), 100 (Cu) and 77 ng L -1 (Zn) for 60 s preconcentration time, at a sample flow rate of 7.0 mL min -1 . Enrichment factors were 102, 91 and 62, for cadmium, copper and zinc, respectively. The procedure has been applied successfully to metal determination in biological standard reference materials

  17. 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.

  18. Advanced steel reheat furnace

    Energy Technology Data Exchange (ETDEWEB)

    Moyeda, D.; Sheldon, M.; Koppang, R. [Energy and Environmental Research Corp., Irvine, CA (United States); Lanyi, M.; Li, X.; Eleazer, B. [Air Products and Chemicals, Inc., Allentown, PA (United States)

    1997-10-01

    Energy and Environmental Research Corp. (EER) under a contract from the Department of Energy is pursuing the development and demonstration of an Advanced Steel Reheating Furnace. This paper reports the results of Phase 1, Research, which has evaluated an advanced furnace concept incorporating two proven and commercialized technologies previously applied to other high temperature combustion applications: EER`s gas reburn technology (GR) for post combustion NOx control; and Air Product`s oxy-fuel enrichment air (OEA) for improved flame heat transfer in the heating zones of the furnace. The combined technologies feature greater production throughput with associated furnace efficiency improvements; lowered NOx emissions; and better control over the furnace atmosphere, whether oxidizing or reducing, leading to better control over surface finish.

  19. 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.

  20. 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 HQ cloud point 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.

  1. Artificial graphites

    International Nuclear Information System (INIS)

    Maire, J.

    1984-01-01

    Artificial graphites are obtained by agglomeration of carbon powders with an organic binder, then by carbonisation at 1000 0 C and graphitization at 2800 0 C. After description of the processes and products, we show how the properties of the various materials lead to the various uses. Using graphite enables us to solve some problems, but it is not sufficient to satisfy all the need of the application. New carbonaceous material open application range. Finally, if some products are becoming obsolete, other ones are being developed in new applications [fr

  2. Model based energy benchmarking for glass furnace

    International Nuclear Information System (INIS)

    Sardeshpande, Vishal; Gaitonde, U.N.; Banerjee, Rangan

    2007-01-01

    Energy benchmarking of processes is important for setting energy efficiency targets and planning energy management strategies. Most approaches used for energy benchmarking are based on statistical methods by comparing with a sample of existing plants. This paper presents a model based approach for benchmarking of energy intensive industrial processes and illustrates this approach for industrial glass furnaces. A simulation model for a glass furnace is developed using mass and energy balances, and heat loss equations for the different zones and empirical equations based on operating practices. The model is checked with field data from end fired industrial glass furnaces in India. The simulation model enables calculation of the energy performance of a given furnace design. The model results show the potential for improvement and the impact of different operating and design preferences on specific energy consumption. A case study for a 100 TPD end fired furnace is presented. An achievable minimum energy consumption of about 3830 kJ/kg is estimated for this furnace. The useful heat carried by glass is about 53% of the heat supplied by the fuel. Actual furnaces operating at these production scales have a potential for reduction in energy consumption of about 20-25%

  3. Porous (Swiss-Cheese Graphite

    Directory of Open Access Journals (Sweden)

    Joseph P. Abrahamson

    2018-05-01

    Full Text Available Porous graphite was prepared without the use of template by rapidly heating the carbonization products from mixtures of anthracene, fluorene, and pyrene with a CO2 laser. Rapid CO2 laser heating at a rate of 1.8 × 106 °C/s vaporizes out the fluorene-pyrene derived pitch while annealing the anthracene coke. The resulting structure is that of graphite with 100 nm spherical pores. The graphitizablity of the porous material is the same as pure anthracene coke. Transmission electron microscopy revealed that the interfaces between graphitic layers and the pore walls are unimpeded. Traditional furnace annealing does not result in the porous structure as the heating rates are too slow to vaporize out the pitch, thereby illustrating the advantage of fast thermal processing. The resultant porous graphite was prelithiated and used as an anode in lithium ion capacitors. The porous graphite when lithiated had a specific capacity of 200 mAh/g at 100 mA/g. The assembled lithium ion capacitor demonstrated an energy density as high as 75 Wh/kg when cycled between 2.2 V and 4.2 V.

  4. Raman characterization of bulk ferromagnetic nanostructured graphite

    International Nuclear Information System (INIS)

    Pardo, Helena; Divine Khan, Ngwashi; Faccio, Ricardo; Araújo-Moreira, F.M.; Fernández-Werner, Luciana

    2012-01-01

    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 -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.

  5. Comparison of a burning mass ceramics coating in laboratory furnace and instrustrial furnace

    International Nuclear Information System (INIS)

    Soares, R.A.L.; Castro, J.R. de S.

    2012-01-01

    This work intends to analyze the differences obtained in the technological properties of a ceramic coating after firing in two distinct environments, laboratory furnace and industrial furnace. For this, was characterized a ceramic mass used in the production of porous coating. The analyzes were performed chemical, mineralogical and thermal mass in that. The specimens were obtained by compacting and burned in the maximum temperature of 1140 deg C in two furnaces, laboratory and industrial. The technological tests were performed linear shrinkage, water absorption, bulk density and mechanical strength. The microstructure was evaluated by ray-X diffraction and scanning electron microscopy. The results showed that both furnaces provided significant differences in analyzed specimens, such as increased strength and low water absorption in the fired samples in a laboratory furnace, for example. (author)

  6. 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

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

    International Nuclear Information System (INIS)

    Soelberg, N.R.; Chambers, A.G.; Ball, L.

    1995-01-01

    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

  8. High Temperature Transparent Furnace Development

    Science.gov (United States)

    Bates, Stephen C.

    1997-01-01

    This report describes the use of novel techniques for heat containment that could be used to build a high temperature transparent furnace. The primary objective of the work was to experimentally demonstrate transparent furnace operation at 1200 C. Secondary objectives were to understand furnace operation and furnace component specification to enable the design and construction of a low power prototype furnace for delivery to NASA in a follow-up project. The basic approach of the research was to couple high temperature component design with simple concept demonstration experiments that modify a commercially available transparent furnace rated at lower temperature. A detailed energy balance of the operating transparent furnace was performed, calculating heat losses through the furnace components as a result of conduction, radiation, and convection. The transparent furnace shells and furnace components were redesigned to permit furnace operation at at least 1200 C. Techniques were developed that are expected to lead to significantly improved heat containment compared with current transparent furnaces. The design of a thermal profile in a multizone high temperature transparent furnace design was also addressed. Experiments were performed to verify the energy balance analysis, to demonstrate some of the major furnace improvement techniques developed, and to demonstrate the overall feasibility of a high temperature transparent furnace. The important objective of the research was achieved: to demonstrate the feasibility of operating a transparent furnace at 1200 C.

  9. 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.

  10. Selective determination of four arsenic species in rice and water samples by modified graphite electrode-based electrolytic hydride generation coupled with atomic fluorescence spectrometry.

    Science.gov (United States)

    Yang, Xin-An; Lu, Xiao-Ping; Liu, Lin; Chi, Miao-Bin; Hu, Hui-Hui; Zhang, Wang-Bing

    2016-10-01

    This work describes a novel non-chromatographic approach for the accurate and selective determining As species by modified graphite electrode-based electrolytic hydride generation (EHG) for sample introduction coupled with atomic fluorescence spectrometry (AFS) detection. Two kinds of sulfydryl-containing modifiers, l-cysteine (Cys) and glutathione (GSH), are used to modify cathode. The EHG performance of As has been changed greatly at the modified cathode, which has never been reported. Arsenite [As(III)] on the GSH modified graphite electrode (GSH/GE)-based EHG can be selectively and quantitatively converted to AsH3 at applied current of 0.4A. As(III) and arsenate [As(V)] on the Cys modified graphite electrode (Cys/GE) EHG can be selectively and efficiently converted to arsine at applied current of 0.6A, whereas monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA) do not form any or only less volatile hydrides under this condition. By changing the analytical conditions, we also have achieved the analysis of total As (tAs) and DMA. Under the optimal condition, the detection limits (3s) of As(III), iAs and tAs in aqueous solutions are 0.25μgL(-1), 0.22μgL(-1) and 0.10μgL(-1), respectively. The accuracy of the method is verified through the analysis of standard reference materials (SRM 1568a). Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Specific features of direct formation of graphite-like microstructures in polycarbonate samples by single femtosecond laser pulses

    Energy Technology Data Exchange (ETDEWEB)

    Ganin, D V; Lapshin, K E; Obidin, A Z; Vartapetov, S K [Physics Instrumentation Center, A.M. Prokhorov General Physics Institute, Russian Academy of Sciences, Troitsk, Moscow Region (Russian Federation)

    2015-11-30

    We present the result of the experiments on producing graphite-like cylindrical microstructures by focusing single femtosecond laser pulses into the bulk of a transparent polymer (polycarbonate). The microstructures are embedded in a cladding with a modified refractive index, possessing waveguide properties. In the experiments with nontransparent screens and diaphragms, placed in the laser beam in front of the entrance pupil of the objective with a large numerical aperture, we have found that the paraxial rays are blocked by the peripheral ones, which reduces the length of the destruction region in the pre-focal zone. In the experiments with transparent screens and diaphragms, introducing optical delays τ{sub d} between the paraxial and peripheral rays, the quantitative dependence of the destruction region length in the pre-focal zone on the value of τ{sub d} is determined. (interaction of laser radiation with matter. laser plasma)

  12. Characterization of core-drilled cokes in a working blast furnace

    Energy Technology Data Exchange (ETDEWEB)

    Shanning Dong; Nigel Paterson; Denis R. Dugwell; Rafael Kandiyoti [Imperial College London, London (United Kingdom). Dept. of Chemical Engineering

    2007-07-01

    A batch of tuyere-level core-drilled cokes, taken from a blast furnace working with coal injection has been characterized using a battery of analytical techniques. These included size exclusion chromatography (SEC), FT-Raman Spectroscopy (FT-RS) and X-ray Powder Diffraction (XRD). SEC tests on NMP-extracts of cokes taken from zones where temperatures were ca. 1500{sup o}C, showed the presence of heavy soot-like material (ca. 107-108 u apparent mass). By contrast, cokes in higher temperature zones (ca. 2000{sup o}C), only gave small amounts of extractable material with up to ca. 105 u apparent mass. The presence of soot-like material indicated the conversion-unfavoured locations at the tuyere-level. FT-Raman spectra of NMP-extracted cokes varied: the area ratios of D (at 1288-1295cm{sup -1}) to G (at ca. 1596cm{sup -1}) bands decreased as the exposure temperature increased. The random (r) fractions decreased with increasing exposure temperature, whereas, the graphitic (G) fractions increased whilst the defect (D) fraction showed a more complex variation with temperature. The latter is a likely indicator of graphitization of tuyere-level cokes in the blast furnace. The Raman spectral results were validated by XRD analyses of the demineralised and NMP-extracted cokes. Raceway coke possessed the largest crystalline dimensions and closest inter-layer spacing because it had encountered highest temperatures as well as iron catalysis. The combination of SEC and Raman spectrometry on core-drill samples has provided information relevant for maintaining stable operation in a blast-furnace operating with coal injection. 13 refs., 7 figs., 6 tabs.

  13. Purification and preparation of graphite oxide from natural graphite

    Energy Technology Data Exchange (ETDEWEB)

    Panatarani, C., E-mail: c.panatarani@phys.unpad.ac.id; Muthahhari, N.; Joni, I. Made [Instrumentation Systems and Functional Material Processing Laboratory, Department of Physics, Faculty of Mathematics and Natural Sciences, Universitas Padjadjaran, Padjadjaran University, Jl. Raya Bandung-Sumedang KM 21, Jatinangor, 45363, Jawa Barat (Indonesia); Rianto, Anton [Grafindo Nusantara Ltd., Belagio Mall Lantai 2, Unit 0 L3-19, Kawasan Mega Kuningan, Kav. B4 No.3, Jakarta Selatan (Indonesia)

    2016-03-11

    Graphite oxide has attracted much interest as a possible route for preparation of natural graphite in the large-scale production and manipulation of graphene as a material with extraordinary electronic properties. Graphite oxide was prepared by modified Hummers method from purified natural graphite sample from West Kalimantan. We demonstrated that natural graphite is well-purified by acid leaching method. The purified graphite was proceed for intercalating process by modifying Hummers method. The modification is on the reaction time and temperature of the intercalation process. The materials used in the intercalating process are H{sub 2}SO{sub 4} and KMNO{sub 4}. The purified natural graphite is analyzed by carbon content based on Loss on Ignition test. The thermo gravimetricanalysis and the Fouriertransform infrared spectroscopy are performed to investigate the oxidation results of the obtained GO which is indicated by the existence of functional groups. In addition, the X-ray diffraction and energy dispersive X-ray spectroscopy are also applied to characterize respectively for the crystal structure and elemental analysis. The results confirmed that natural graphite samples with 68% carbon content was purified into 97.68 % carbon content. While the intercalation process formed a formation of functional groups in the obtained GO. The results show that the temperature and reaction times have improved the efficiency of the oxidation process. It is concluded that these method could be considered as an important route for large-scale production of graphene.

  14. A simple and sensitive methodology for voltammetric determination of valproic acid in human blood plasma samples using 3-aminopropyletriethoxy silane coated magnetic nanoparticles modified pencil graphite electrode.

    Science.gov (United States)

    Zabardasti, Abedin; Afrouzi, Hossein; Talemi, Rasoul Pourtaghavi

    2017-07-01

    In this work, we have prepared a nano-material modified pencil graphite electrode for the sensing of valproic acid (VA) by immobilization 3-aminopropyletriethoxy silane coated magnetic nanoparticles (APTES-MNPs) on the pencil graphite surface (PGE). Electrochemical studies indicated that the APTES-MNPs efficiently increased the electron transfer kinetics between VA and the electrode and the free NH 2 groups of the APTES on the outer surface of magnetic nanoparticles can interact with carboxyl groups of VA. Based on this, we have proposed a sensitive, rapid and convenient electrochemical method for VA determination. Under the optimized conditions, the reduction peak current of VA is found to be proportional to its concentration in the range of 1.0 (±0.2) to 100.0 (±0.3) ppm with a detection limit of 0.4 (±0.1) ppm. The whole sensor fabrication process was characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) methods with using [Fe(CN) 6 ] 3-/4- as an electrochemical redox indicator. The prepared modified electrode showed several advantages such as high sensitivity, selectivity, ease of preparation and good repeatability, reproducibility and stability. The proposed method was applied to determination of valproic acid in blood plasma samples and the obtained results were satisfactory accurate. Copyright © 2017. Published by Elsevier B.V.

  15. Acoustic Levitator With Furnace And Laser Heating

    Science.gov (United States)

    Barmatz, Martin B.; Stoneburner, James D.

    1991-01-01

    Acoustic-levitation apparatus incorporates electrical-resistance furnace for uniform heating up to temperature of about 1,000 degrees C. Additional local heating by pair of laser beams raise temperature of sample to more than 1,500 degrees C. High temperature single-mode acoustic levitator generates cylindrical-mode accoustic resonance levitating sample. Levitation chamber enclosed in electrical-resistance furnace. Infrared beams from Nd:YAG laser provide additional local heating of sample. Designed for use in containerless processing of materials in microgravity or in normal Earth gravity.

  16. A graphite foam reinforced by graphite particles

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, J.J.; Wang, X.Y.; Guo, L.F.; Wang, Y.M.; Wang, Y.P.; Yu, M.F.; Lau, K.T.T. [DongHua University, Shanghai (China). College of Material Science and Engineering

    2007-11-15

    Graphite foam was obtained after carbonization and graphitization of a pitch foam formed by the pyrolysis of coal tar based mesophase pitch mixed with graphite particles in a high pressure and temperature chamber. The graphite foam possessed high mechanical strength and exceptional thermal conductivity after adding the graphite particles. Experimental results showed that the thermal conductivity of modified graphite foam reached 110W/m K, and its compressive strength increased from 3.7 MPa to 12.5 MPa with the addition of 5 wt% graphite particles. Through the microscopic observation, it was also found that fewer micro-cracks were formed in the cell wall of the modified foam as compared with pure graphite foam. The graphitization degree of modified foam reached 84.9% and the ligament of graphite foam exhibited high alignment after carbonization at 1200{sup o}C for 3 h and graphitization at 3000{sup o}C for 10 min.

  17. Atomic absorption determination of ultratrace tellurium in rocks utilizing high sensitivity sampling systems

    International Nuclear Information System (INIS)

    Beaty, R.D.

    1973-01-01

    The sampling boat and the graphite furnace were shown to possess the required sensitivity to detect tellurium at ultratrace levels, in a variety of sample types, by atomic absorption. In the sampling boat approach, tellurium in sample solutions is chemically separated and concentrated by extraction into methyl isobutyl ketone before measurement. For samples exhibiting extraction interferences or excessively high background absorption, a preliminary separation of tellurium by coprecipitation with selenium is described. Using this technique, tellurium can be quantitatively detected down to 5 nanograms and linear response is observed to 100 nanograms. Relative standard deviations of better than 7 percent are achieved for 50 nanograms of tellurium. For samples that have a tellurium content below the detection limits of the sampling boat, the graphite furnace is used for atomization. By this method, as little as 0.07 nanograms of tellurium can be detected, and a precision of 1 percent relative standard deviation is achievable at the 5 nanogram level. A routinely applicable procedure was developed for determining tellurium in rocks, using the graphite furnace, after a hydrofluoric acid decomposition of the sample. Using this procedure, tellurium data were obtained on 20 different rocks, and the significance of this new information is discussed. (Diss. Abstr. Int., B)

  18. 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.

  19. Determination of element concentrations in biological reference materials by solid sampling and other analytical methods

    International Nuclear Information System (INIS)

    Schauenburg, H.; Weigert, P.

    1992-01-01

    Using solid sampling with graphite furnace atomic absorption spectrometry (GFAAS), values for cadmium, copper, lead and zinc in six biological reference materials were obtained from up to four laboratories participating in three collaborative studies. These results are compared with those obtained with other methods used in routine analysis from laboratories of official food control. Under certain conditions solid sampling with GFAAS seems to be suitable for routine analysis as well as conventional methods. (orig.)

  20. 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.

  1. Characterisation of Chlorine Behavior in French Graphite

    International Nuclear Information System (INIS)

    Blondel, A.; Moncoffre, N.; Toulhoat, N.; Bererd, N.; Petit, L.; Laurent, G.; Lamouroux, C.

    2016-01-01

    Chlorine 36 is one of the main radionuclides of concern for French graphite waste disposal. In order to help the understanding of its leaching behaviour under disposal conditions, the respective impact of temperature, irradiation and gas radiolysis on chlorine release in reactor has been studied. Chlorine 36 has been simulated through chlorine 37 ion implantation in virgin nuclear graphite samples. Results show that part of chlorine is highly mobile in graphite in the range of French reactors operating temperatures in relation with graphite structural recovering. Ballistic damage generated by irradiation also promotes chlorine release whereas no clear impact of the coolant gas radiolysis was observed in the absence of graphite radiolytic corrosion. (author)

  2. Steam generators and furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Swoboda, E

    1978-04-01

    The documents published in 1977 in the field of steam generators for conventional thermal power plants are classified according to the following subjects: power industry and number of power plants, planning and operation, design and construction, furnaces, environmental effects, dirt accumulation and corrosion, conservation and scouring, control and automation, fundamental research, and materials.

  3. Harwell Graphite Calorimeter

    International Nuclear Information System (INIS)

    Linacre, J.K.

    1970-01-01

    The calorimeter is of the steady state temperature difference type. It contains a graphite sample supported axially in a graphite outer jacket, the assembly being contained in a thin stainless steel outer can. The temperature of the jacket and the temperature difference between sample and jacket are measured by chromel-alumel thermocouples. The instrument is calibrated by means of an electric heater of low mass positioned on the axis of the sample. The resistance of the heater is known and both current through the heater and the potential across it may be measured. The instrument is filled with nitrogen at a pressure of one half atmosphere at room temperature. The calorimeter has been designed for prolonged operation at temperatures up to 600°C, and dose rates up to 1 Wg -1 , and instruments have been in use for periods in excess of one year

  4. 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.

  5. 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.

  6. 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.

  7. Electronic properties of graphite

    International Nuclear Information System (INIS)

    Schneider, J.

    2010-10-01

    In this thesis, low-temperature magneto-transport (T ∼ 10 mK) and the de Haas-van Alphen effect of both natural graphite and highly oriented pyrolytic graphite (HOPG) are examined. In the first part, low field magneto-transport up to B = 11 T is discussed. A Fourier analysis of the background removed signal shows that the electric transport in graphite is governed by two types of charge carriers, electrons and holes. Their phase and frequency values are in agreement with the predictions of the SWM-model. The SWM-model is confirmed by detailed band structure calculations using the magnetic field Hamiltonian of graphite. The movement of the Fermi at B > 2 T is calculated self-consistently assuming that the sum of the electron and hole concentrations is constant. The second part of the thesis deals with high field magneto-transport of natural graphite in the magnetic field range 0 ≤ B ≤ 28 T. Both spin splitting of magneto-transport features in tilted field configuration and the onset of the charge density wave (CDW) phase for different temperatures with the magnetic field applied normal to the sample plane are discussed. Concerning the Zeeman effect, the SWM calculations including the Fermi energy movement require a g-factor of g* equal to 2.5 ± 0.1 to reproduce the spin spilt features. The measurements of the charge density wave state confirm that its onset magnetic field can be described by a Bardeen-Cooper-Schrieffer (BCS)-type formula. The measurements of the de Haas-van Alphen effect are in agreement with the results of the magneto-transport measurements at low field. (author)

  8. Online combination of reversed-phase/reversed-phase and porous graphitic carbon liquid chromatography for multicomponent separation of proteomics and glycoproteomics samples.

    Science.gov (United States)

    Lam, Maggie P Y; Lau, Edward; Siu, S O; Ng, Dominic C M; Kong, Ricky P W; Chiu, Philip C N; Yeung, William S B; Lo, Clive; Chu, Ivan K

    2011-11-01

    In this paper, we describe an online combination of reversed-phase/reversed-phase (RP-RP) and porous graphitic carbon (PGC) liquid chromatography (LC) for multicomponent analysis of proteomics and glycoproteomics samples. The online RP-RP portion of this system provides comprehensive 2-D peptide separation based on sequence hydrophobicity at pH 2 and 10. Hydrophilic components (e.g. glycans, glycopeptides) that are not retained by RP are automatically diverted downstream to a PGC column for further trapping and separation. Furthermore, the RP-RP/PGC system can provide simultaneous extension of the hydropathy range and peak capacity for analysis. Using an 11-protein mixture, we found that the system could efficiently separate native peptides and released N-glycans from a single sample. We evaluated the applicability of the system to the analysis of complex biological samples using 25 μg of the lysate of a human choriocarcinoma cell line (BeWo), confidently identifying a total of 1449 proteins from a single experiment and up to 1909 distinct proteins from technical triplicates. The PGC fraction increased the sequence coverage through the inclusion of additional hydrophilic sequences that accounted for up to 6.9% of the total identified peptides from the BeWo lysate, with apparent preference for the detection of hydrophilic motifs and proteins. In addition, RP-RP/PGC is applicable to the analysis of complex glycomics samples, as demonstrated by our analysis of a concanavalin A-extracted glycoproteome from human serum; in total, 134 potentially N-glycosylated serum proteins, 151 possible N-glycosylation sites, and more than 40 possible N-glycan structures recognized by concanavalin A were simultaneously detected. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Process for purifying graphite

    International Nuclear Information System (INIS)

    Clausius, R.A.

    1985-01-01

    A process for purifying graphite comprising: comminuting graphite containing mineral matter to liberate at least a portion of the graphite particles from the mineral matter; mixing the comminuted graphite particles containing mineral matter with water and hydrocarbon oil to form a fluid slurry; separating a water phase containing mineral matter and a hydrocarbon oil phase containing grahite particles; and separating the graphite particles from the hydrocarbon oil to obtain graphite particles reduced in mineral matter. Depending upon the purity of the graphite desired, steps of the process can be repeated one or more times to provide a progressively purer graphite

  10. 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.

  11. Volatilization-excitation phenomena and efficiency of spectrochemical buffers in the analysis of geological samples. I. The action of the mixture Li2CO3: graphite

    International Nuclear Information System (INIS)

    Diaz-Guerra, J.P.; Roca, M.

    1984-01-01

    The volatilization-excitation mechanisms of Li 2 CO 3 , SrCO 3 and GeO 2 as buffers for the determination of different major constituents in geological samples have been investigated considering the phenomena taking place in the electrode, anodic load and arc plasma. The present paper deals with the evaluation of fundamental parameters and processes in d.c. arc that have first been applied to the study of a Li 2 CO 3 : graphite (1:1) mixture. A second paper is devoted to ascertain the action of each of the other two species. Intensity-time curves, variation of voltage between the electrodes, vapour diffusion through the electrode wall, load depletion, reaction products formation, and temperature, electron pressure and ionization degree in the arc plasma have been studied. The measurement of plasma parameters has been performed by introducing thermometric and manometric species in both the anode and the cathode electrodes. A procedure for calculating the relative emission efficiencies of the analytical lines, taking into account the transportation process, has been developed. (author)

  12. 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

  13. 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.

  14. 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.

  15. 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)

  16. Blast furnace hearth lining: post mortem analysis

    International Nuclear Information System (INIS)

    Almeida, Bruno Vidal de; Vernilli Junior, Fernando

    2017-01-01

    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"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)

  17. Formation mechanism of the protective layer in a blast furnace hearth

    Science.gov (United States)

    Jiao, Ke-xin; Zhang, Jian-liang; Liu, Zheng-jian; Xu, Meng; Liu, Feng

    2015-10-01

    A variety of techniques, such as chemical analysis, scanning electron microscopy-energy dispersive spectroscopy, and X-ray diffraction, were applied to characterize the adhesion protective layer formed below the blast furnace taphole level when a certain amount of titanium- bearing burden was used. Samples of the protective layer were extracted to identify the chemical composition, phase assemblage, and distribution. Furthermore, the formation mechanism of the protective layer was determined after clarifying the source of each component. Finally, a technical strategy was proposed for achieving a stable protective layer in the hearth. The results show that the protective layer mainly exists in a bilayer form in the sidewall, namely, a titanium-bearing layer and a graphite layer. Both the layers contain the slag phase whose major crystalline phase is magnesium melilite (Ca2MgSi2O7) and the main source of the slag phase is coke ash. It is clearly determined that solid particles such as graphite, Ti(C,N) and MgAl2O4 play an important role in the formation of the protective layer, and the key factor for promoting the formation of a stable protective layer is reasonable control of the evolution behavior of coke.

  18. Glass: Rotary Electric Glass Furnace

    Energy Technology Data Exchange (ETDEWEB)

    Recca, L.

    1999-01-29

    Compared to conventional gas-fired furnaces, the new rotary electric furnace will increase energy efficiency while significantly reducing air emissions, product turnaround time, and labor costs. As this informative new fact sheet explains, the thousand different types of glass optical blanks produced for the photonics industry are used for lasers, telescopes, cameras, lights, and many other products.

  19. 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.

  20. 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...

  1. Sample preparation in alkaline media

    International Nuclear Information System (INIS)

    Nobrega, Joaquim A.; Santos, Mirian C.; Sousa, Rafael A. de; Cadore, Solange; Barnes, Ramon M.; Tatro, Mark

    2006-01-01

    The use of tetramethylammonium hydroxide, tertiary amines and strongly alkaline reagents for sample treatment involving extraction and digestion procedures is discussed in this review. The preparation of slurries is also discussed. Based on literature data, alkaline media offer a good alternative for sample preparation involving an appreciable group of analytes in different types of samples. These reagents are also successfully employed in tailored speciation procedures wherein there is a critical dependence on maintenance of chemical forms. The effects of these reagents on measurements performed using spectroanalytical techniques are discussed. Several undesirable effects on transport and atomization processes necessitate use of the method of standard additions to obtain accurate results. It is also evident that alkaline media can improve the performance of techniques such as inductively coupled plasma mass spectrometry and accessories, such as autosamplers coupled to graphite furnace atomic absorption spectrometers

  2. Phonon scattering in graphite

    International Nuclear Information System (INIS)

    Wagner, P.

    1976-04-01

    Effects on graphite thermal conductivities due to controlled alterations of the graphite structure by impurity addition, porosity, and neutron irradiation are shown to be consistent with the phonon-scattering formulation 1/l = Σ/sub i equals 1/sup/n/ 1/l/sub i/. Observed temperature effects on these doped and irradiated graphites are also explained by this mechanism

  3. 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.

  4. Furnace for treating bituminous material

    Energy Technology Data Exchange (ETDEWEB)

    Klotzer, M

    1922-04-28

    A furnace with saw-teeth-like profiled hearth, which by means of a kind of shaking slide executes a backward and forward motion, for carrying out the process according to Patent 422,391. It is characterized in that the stroke of the hearth moving in the furnace is smaller than the length of the profile tooth and the height of the feed is held less than the tooth height.

  5. 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.

  6. Ion irradiated graphite exposed to fusion-relevant deuterium plasma

    International Nuclear Information System (INIS)

    Deslandes, Alec; Guenette, Mathew C.; Corr, Cormac S.; Karatchevtseva, Inna; Thomsen, Lars; Ionescu, Mihail; Lumpkin, Gregory R.; Riley, Daniel P.

    2014-01-01

    Graphite samples were irradiated with 5 MeV carbon ions to simulate the damage caused by collision cascades from neutron irradiation in a fusion environment. The ion irradiated graphite samples were then exposed to a deuterium plasma in the linear plasma device, MAGPIE, for a total ion fluence of ∼1 × 10 24 ions m −2 . Raman and near edge X-ray absorption fine structure (NEXAFS) spectroscopy were used to characterize modifications to the graphitic structure. Ion irradiation was observed to decrease the graphitic content and induce disorder in the graphite. Subsequent plasma exposure decreased the graphitic content further. Structural and surface chemistry changes were observed to be greatest for the sample irradiated with the greatest fluence of MeV ions. D retention was measured using elastic recoil detection analysis and showed that ion irradiation increased the amount of retained deuterium in graphite by a factor of four

  7. 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.

  8. Methane generated from graphite--tritium interaction

    International Nuclear Information System (INIS)

    Coffin, D.O.; Walthers, C.R.

    1979-01-01

    When hydrogen isotopes are separated by cryogenic distillation, as little as 1 ppM of methane will eventually plug the still as frost accumulates on the column packings. Elemental carbon exposed to tritium generates methane spontaneously, and yet some dry transfer pumps, otherwise compatible with tritium, convey the gas with graphite rotors. This study was to determine the methane production rate for graphite in tritium. A pump manufacturer supplied graphite samples that we exposed to tritium gas at 0.8 atm. After 137 days we measured a methane synthesis rate of 6 ng/h per cm 2 of graphite exposed. At this rate methane might grow to a concentration of 0.01 ppM when pure tritium is transferred once through a typical graphite--rotor transfer pump. Such a low methane level will not cause column blockage, even if the cryogenic still is operated continuously for many years

  9. 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.

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

    International Nuclear Information System (INIS)

    Liapis, Ioannis; Papayianni, Ioanna

    2015-01-01

    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 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

  11. 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.

  12. Development of vacuum brazing furnace

    International Nuclear Information System (INIS)

    Singh, Rajvir; Yedle, Kamlesh; Jain, A.K.

    2005-01-01

    In joining of components where welding process is not possible brazing processes are employed. Value added components, high quality RF systems, UHV components of high energy accelerators, carbide tools etc. are produced using different types of brazing methods. Furnace brazing under vacuum atmosphere is the most popular and well accepted method for production of the above mentioned components and systems. For carrying out vacuum brazing successfully it is essential to have a vacuum brazing furnace with latest features of modern vacuum brazing technology. A vacuum brazing furnace has been developed and installed for carrying out brazing of components of copper, stainless steel and components made of dissimilar metals/materials. The above furnace has been designed to accommodate jobs of 700mm diameter x 2000mm long sizes with job weight of 500kgs up to a maximum temperature of 1250 degC at a vacuum of 5 x 10 -5 Torr. Oil diffusion pumping system with a combination of rotary and mechanical booster pump have been employed for obtaining vacuum. Molybdenum heating elements, radiation shield of molybdenum and Stainless Steel Grade 304 have been used. The above furnace is computer controlled with manual over ride facility. PLC and Pentium PC are integrated together to maneuver steps of operation and safety interlocks of the system. Closed loop water supply provides cooling to the system. The installation of the above system is in final stage of completion and it will be ready for use in next few months time. This paper presents insights of design and fabrication of a modern vacuum brazing furnace and its sub-system. (author)

  13. Radiolytic graphite oxidation revisited

    International Nuclear Information System (INIS)

    Minshall, P.C.; Sadler, I.A.; Wickham, A.J.

    1996-01-01

    The importance of radiolytic oxidation in graphite-moderated CO 2 -cooled reactors has long been recognised, especially in the Advanced Gas-Cooled Reactors where potential rates are higher because of the higher gas pressure and ratings than the earlier Magnox designs. In all such reactors, the rate of oxidation is partly inhibited by the CO produced in the reaction and, in the AGR, further reduced by the deliberate addition of CH 4 . Significant roles are also played by H 2 and H 2 O. This paper reviews briefly the mechanisms of these processes and the data on which they are based. However, operational experience has demonstrated that these basic principles are unsatisfactory in a number of respects. Gilsocarbon graphites produced by different manufacturers have demonstrated a significant difference in oxidation rate despite a similar specification and apparent equivalence in their pore size and distribution, considered to be the dominant influence on oxidation rate for a given coolant-gas composition. Separately, the inhibiting influence of CH 4 , which for many years had been considered to arise from the formation of a sacrificial deposit on the pore walls, cannot adequately be explained by the actual quantities of such deposits found in monitoring samples which frequently contain far less deposited carbon than do samples from Magnox reactors where the only source of such deposits is the CO. The paper also describes the current status of moderator weight-loss predictions for Magnox and AGR Moderators and the validation of the POGO and DIFFUSE6 codes respectively. 2 refs, 5 figs

  14. 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....

  15. 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.

  16. 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.

  17. Crystallization degree change of expanded graphite by milling and annealing

    International Nuclear Information System (INIS)

    Tang Qunwei; Wu Jihuai; Sun Hui; Fang Shijun

    2009-01-01

    Expanded graphite was ball milled with a planetary mill in air atmosphere, and subsequently thermal annealed. The samples were characterized by using X-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM) and thermal gravimetric analysis (TGA). It was found that in the milling initial stage (less than 12 h), the crystallization degree of the expanded graphite declined gradually, but after milling more than 16 h, a recrystallization of the expanded graphite toke place, and ordered nanoscale expanded graphite was formed gradually. In the annealing initial stage, the non-crystallization of the graphite occurred, but, beyond an annealing time, recrystallizations of the graphite arise. Higher annealing temperature supported the recrystallization. The milled and annealed expanded graphite still preserved the crystalline structure as raw material and hold high thermal stability.

  18. Automated, High Temperature Furnace for Glovebox Operation

    International Nuclear Information System (INIS)

    Neikirk, K.

    2001-01-01

    The Plutonium Immobilization Project (PIP), to be located at the Savannah River Site SRS, is a combined development and testing effort by Lawrence Livermore National Laboratory (LLNL), Westinghouse Savannah River Company (WSRC), Pacific Northwest National Laboratory (PNNL), Argonne National Laboratory (ANL), and the Australian National Science and Technology Organization (ANSTO). The Plutonium Immobilization process involves the disposition of excess plutonium by incorporation into ceramic pucks. As part of the immobilization process, furnaces are needed for sintering the ceramic pucks. The furnace being developed for puck sintering is an automated, bottom loaded furnace with insulating package and resistance heating elements located within a nuclear glovebox. Other furnaces types considered for the application include retort furnaces and pusher furnaces. This paper, in part, will discuss the furnace technologies considered and furnace technology selected to support reliable puck sintering in a glovebox environment

  19. Design of a rotating-hearth furnace

    Energy Technology Data Exchange (ETDEWEB)

    Behrens, H A [Verein Deutscher Eisenhuettenleute (VDEh), Duesseldorf (Germany, F.R.)

    1979-10-01

    Presented in two parts, this paper is intended to provide an outline of the theoretical fundamentals for the design of rotating-hearth furnaces for heating round stock and deals with the characteristic design features of such furnaces.

  20. Waste and dust utilisation in shaft furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Senk, D.; Babich, A.; Gudenau, H.W. [Rhein Westfal TH Aachen, Aachen (Germany)

    2005-07-01

    Wastes and dusts from steel industry, non-ferrous metallurgy and other branches can be utilised e.g. in agglomeration processes (sintering, pelletising 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 pulverised 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.

  1. Study by electronic microscopy of corrosion features of graphite after hot oxidation (air, 620 C)

    International Nuclear Information System (INIS)

    Jodon de Villeroche, Suzanne

    1968-01-01

    The author reports the study of corrosion features of graphite after hot oxidation in the air at 620 C. It is based on observations made by electronic microscopy. This study comes after another one dedicated to oxidation features obtained by hot corrosion of natural graphite, and aims at comparing pyrolytic graphite before and after irradiation in an atomic pile, and at performing tests on a graphite processed with ozone. After a recall of generalities about natural graphite and of some issues related to hot corrosion of natural graphite, the author presents some characteristics and features of irradiated and non-irradiated pyrolytic graphite. He reports the study of the oxidation of samples of pyrolytic graphite: production of thin lamellae, production of glaze-carbon replicates, oxidation of irradiated and of non-irradiated graphite, healing of irradiation defects, and oxidation of ozone-processed natural graphite [fr

  2. A cylindrical furnace for absorption spectral studies

    Indian Academy of Sciences (India)

    A cylindrical furnace with three heating zones, capable of providing a temperature of 1100°C, has been fabricated to enable recording of absorption spectra of high temperature species. The temperature of the furnace can be controlled to ± 1°C of the set temperature. The salient feature of this furnace is that the material ...

  3. 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.

  4. Graphite targets at LAMPF

    International Nuclear Information System (INIS)

    Brown, R.D.; Grisham, D.L.

    1983-01-01

    Rotating polycrystalline and stationary pyrolytic graphite target designs for the LAMPF experimental area are described. Examples of finite element calculations of temperatures and stresses are presented. Some results of a metallographic investigation of irradiated pyrolytic graphite target plates are included, together with a brief description of high temperature bearings for the rotating targets

  5. Electrochemical treatment of graphite

    Energy Technology Data Exchange (ETDEWEB)

    Podlovilin, V.I.; Egorov, I.M.; Zhernovoj, A.I.

    1983-01-01

    In the course of investigating various modes of electrochemical treatment (ECT) it has been found that graphite anode treatment begins under the ''glow mode''. A behaviour of some marks of graphite with the purpose of ECT technique development in different electrolytes has been tested. Electrolytes have been chosen of three types: highly alkaline (pH 13-14), neutral (pH-Z) and highly acidic (pH 1-2). For the first time parallel to mechanical electroerosion treatment, ECT of graphite and carbon graphite materials previously considered chemically neutral is proposed. ECT of carbon graphite materials has a number of advantages as compared with electroerrosion and mechanical ones with respect to the treatment rate and purity (ronghness) of the surface. A small quantity of sludge (6-8%) under ECT is in highly alkali electrolytes.

  6. Electrochemical treatment of graphite

    International Nuclear Information System (INIS)

    Podlovilin, V.I.; Egorov, I.M.; Zhernovoj, A.I.

    1983-01-01

    In the course of investigating various modes of electroche-- mical treatment (ECT) it has been found that graphite anode treatment begins under the ''glow mode''. A behaviour of some marks of graphite with the purpose of ECT technique development in different electrolytes has been tested. Electrolytes have been chosen of three types: highly alkaline (pH 13-14), neutral (pH-Z) and highly acidic (pH 1-2). For the first time parallel to mechanical electroerosion treatment ECT graphite and carbon graphite materials previously considered chemically neutral is proposed. ECT of carbon graphite materials has a number of advantages as compared with electroerrosion and mechanical ones this is treatment rate and purity (ronghness) of the surface. A sMall quantity of sludge (6-8%) under ECT is in highly alkali electrolytes

  7. Direct determination of Cu, Mn, Pb, and Zn in beer by thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Nascentes, Clesia C.; Kamogawa, Marcos Y.; Fernandes, Kelly G.; Arruda, Marco A.Z.; Nogueira, Ana Rita A.; Nobrega, Joaquim A.

    2005-01-01

    In this work, thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was employed for Cu, Mn, Pb, and Zn determination in beer without any sample digestion. The system was optimized and calibration was based on the analyte addition technique. A sample volume of 300 μl was introduced into the hot Ni tube at a flow-rate of 0.4 ml min -1 using 0.14 mol l -1 nitric acid solution or air as carrier. Different Brazilian beers were directly analyzed after ultrasonic degasification. Results were compared with those obtained by graphite furnace atomic absorption spectrometry (GFAAS). The detection limits obtained for Cu, Mn, Pb, and Zn in aqueous solution were 2.2, 18, 1.6, and 0.9 μg l -1 , respectively. The relative standard deviations varied from 2.7% to 7.3% (n=8) for solutions containing the analytes in the 25-50 μg l -1 range. The concentration ranges obtained for analytes in beer samples were: Cu: 38.0-155 μg l -1 ; Mn: 110-348 μg l -1 , Pb: 13.0-32.9 μg l -1 , and Zn: 52.7-226 μg l -1 . Results obtained by TS-FF-AAS and GFAAS were in agreement at a 95% confidence level. The proposed method is fast and simple, since sample digestion is not required and sensitivity can be improved without using expensive devices. The TS-FF-AAS presented suitable sensitivity for determination of Cu, Mn, Pb, and Zn in the quality control of a brewery

  8. Behavior of coke in large blast furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Nakamura, N

    1978-01-01

    Three blast furnaces were quenched in operation and the contents were examined; the temperature distribution was also measured, using Tempil pellets. The furnaces examined included a low productivity one, which was examined to see what was wrong. Changes in the quality of coke as it descends in the furnace, and coke behavior in the raceway and hearth are reported. The functions required of coke, and the effects of poor coke quality, are explained, together with the coke quality required in large blast furnaces. A theoretical study of the role of coke in large blast furnaces is included.

  9. 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.

  10. Industrial furnace with improved heat transfer

    Energy Technology Data Exchange (ETDEWEB)

    Hoetzl, M.; Lingle, T.M.

    1992-07-07

    This patent describes an industrial furnace for heating work which emits volatiles during heating. It comprises a generally cylindrical, closed end furnace section defining a sealable heat transfer chamber for heating work disposed therein; fan means for directing furnace atmosphere as a swirling wind mass about the interior of the furnace section over a portion thereof; heat means for heating the wind mass within the fan chamber; and an incineration track formed as a circumferentially extending groove about the exterior of the furnace section and in heat transfer relationship with and situated at least to extend about a portion of the fan chamber.

  11. Radiometric report for a blast furnace tracing with radioactive isotopes

    International Nuclear Information System (INIS)

    Tanase, G.; Tanase, M.

    1995-01-01

    One of the methods to monitor refractory wall of blast furnace is its tracing with radioactive isotopes. The tracer isotope can be detected by two ways: the external dosimetric measurement at the armour of the blast furnace and/or the radiometric measurement of the iron sample charge by charge. Any change in radiometric situation of tracer radioisotope is recorded in a radiometric report. This paper presents an original concept of radiometric report based upon PARADOX and CORELDRAW soft kits. Their advantage are: quick and easy changes, easy recording of current radioactivity of tracer isotope, short history of changes, visual mapping of the tracer isotope and others. In this way we monitored 6 blast furnaces and more than 180 radioactive sources

  12. 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.

  13. 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.

  14. Asymptomatic Intracorneal Graphite Deposits following Graphite Pencil Injury

    OpenAIRE

    Philip, Swetha Sara; John, Deepa; John, Sheeja Susan

    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.

  15. Actinides in irradiated graphite of RBMK-1500 reactor

    Energy Technology Data Exchange (ETDEWEB)

    Plukienė, R., E-mail: rita@ar.fi.lt; Plukis, A.; Barkauskas, V.; Gudelis, A.; Gvozdaitė, R.; Duškesas, G.; Remeikis, V.

    2014-10-01

    Highlights: • Activation of actinides in the graphite of the RBMK-1500 reactor was analyzed. • Numerical modeling using SCALE 6.1 and MCNPX was used for actinide calculation. • Measurements of the irradiated graphite sample were used for model validation. • Results are important for further decommissioning process of the RBMK type reactors. - Abstract: The activation of graphite in the nuclear power plants is the problem of high importance related with later graphite reprocessing or disposal. The activation of actinide impurities in graphite due to their toxicity determines a particular long term risk to waste management. In this work the activation of actinides in the graphite constructions of the RBMK-1500 reactor is determined by nuclear spectrometry measurements of the irradiated graphite sample from the Ignalina NPP Unit I and by means of numerical modeling using two independent codes SCALE 6.1 (using TRITON-VI sequence) and MCNPX (v2.7 with CINDER). Both models take into account the 3D RBMK-1500 reactor core fragment with explicit graphite construction including a stack and a sleeve but with a different simplification level concerning surrounding graphite and construction of control roads. The verification of the model has been performed by comparing calculated and measured isotope ratios of actinides. Also good prediction capabilities of the actinide activation in the irradiated graphite have been found for both calculation approaches. The initial U impurity concentration in the graphite model has been adjusted taking into account the experimental results. The specific activities of actinides in the irradiated RBMK-1500 graphite constructions have been obtained and differences between numerical simulation results, different structural parts (sleeve and stack) as well as comparison with previous results (Ancius et al., 2005) have been discussed. The obtained results are important for further decommissioning process of the Ignalina NPP and other RBMK

  16. Multikilowatt variable frequency microwave furnace

    International Nuclear Information System (INIS)

    Bible, D.W.; Lauf, R.J.; Everleigh, C.A.

    1992-01-01

    In this paper, the authors describe a new type of microwave processing furnace in which the frequency can be varied continuously from 4 to 8 GHz and the power level varied from zero up to 2.5 kW. The extraordinary bandwidth of this furnace is achieved by using a traveling wave tube (TWT) amplifier originally developed for electronic warfare applications. The TWT is a linear beam device characterized by a traveling electromagnetic wave that continuously extracts energy longitudinally along the path of an electron beam. The TWT, unlike other microwave tubes such as the magnetron, klystron, gyrotron, and others, does not depend upon resonant RF fields and is therefore capable of wide bandwidth operation.operation

  17. The fate of injectant coal in blast furnaces: The origin of extractable materials of high molecular mass in blast furnace carryover dusts

    Energy Technology Data Exchange (ETDEWEB)

    Dong, S.N.; Wu, L.; Paterson, N.; Herod, A.A.; Dugwell, D.R.; Kandiyoti, R. [University of London Imperial College of Science & Technology, London (United Kingdom). Dept. of Chemical Engineering

    2005-07-01

    The aim of the work was to investigate the fate of injectant coal in blast furnaces and the origin of extractable materials in blast furnace carryover dusts. Two sets of samples including injectant coal and the corresponding carryover dusts from a full sized blast furnace and a pilot scale rig have been examined. The samples were extracted using 1-methyl-2-pyrrolidinone (NMP) solvent and the extracts studied by size exclusion chromatography (SEC). The blast furnace carryover dust extracts contained high molecular weight carbonaceous material, of apparent mass corresponding to 10{sup 7}-10{sup 8} u, by polystyrene calibration. In contrast, the feed coke and char prepared in a wire mesh reactor under high temperature conditions did not give any extractable material. Meanwhile, controlled combustion experiments in a high-pressure wire mesh reactor suggest that the extent of combustion of injectant coal in the blast furnace tuyeres and raceways is limited by time of exposure and very low oxygen concentration. It is thus likely that the extractable, soot-like material in the blast furnace dust originated in tars is released by the injectant coal. Our results suggest that the unburned tars were thermally altered during the upward path within the furnace, giving rise to the formation of heavy molecular weight (soot-like) materials.

  18. Recent developments in graphite

    International Nuclear Information System (INIS)

    Cunningham, J.E.

    1983-01-01

    Overall, the HTGR graphite situation is in excellent shape. In both of the critical requirements, fuel blocks and support structures, adequate graphites are at hand and improved grades are sufficiently far along in truncation. In the aerospace field, GraphNOL N3M permits vehicle performance with confidence in trajectories unobtainable with any other existing material. For fusion energy applications, no other graphite can simultaneously withstand both extreme thermal shock and neutron damage. Hence, the material promises to create new markets as well as to offer a better candidate material for existing applications

  19. Graphite for fusion energy applications

    International Nuclear Information System (INIS)

    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

  20. Recycling of electric arc furnace dust

    International Nuclear Information System (INIS)

    Marques Sobrinho, Vicente de Paulo Ferreira; Oliveira, Jose Roberto de; Tenorio, Jorge Alberto Soares; Espinosa, Denise Crocce Romano

    2010-01-01

    This research aims to study the process of incorporation of the metal iron in electric arc furnace dust (EAFD), from a steel mill producing long steel by liquid iron in addition to the changing temperature of 1400 degrees Celsius of EAFD 'as received', the percentage of EAFD to be added (5, 10 and 20% of initial weight of sample pig iron) and the time of withdrawal of the sample of pig iron and slag (30 minutes after the addition of EAFD). Previously, the EAFD will be characterized using the following techniques: chemical analysis, size analysis, specific surface area, Xray diffraction, scanning electron microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) microanalysis. . After characterization, the EAFD will be added to the bath of liquid pig iron. It is expected that the results obtained at the end of the research allow the evaluation of the iron metal incorporation of EAFD in pig iron bath. (author)

  1. Metal diffusion from furnace tubes depends on location

    International Nuclear Information System (INIS)

    Albright, L.F.

    1988-01-01

    Studies of metal samples from an ethylene furnace on the Texas Gulf Coast, using a scanning electron microscope (SEM) and an energy dispersive X-ray analyzer (EDAX), reveal preferential diffusion of chromium, titanium, and aluminum in the coil wall to the surfaces of the tube where they form metal oxides. These elements are gradually depleted from the tube wall. Complicated surface reactions that include the formation of several metal oxides, metal sulfides, and metal-catalyzed coke also occur. Several mechanisms can be postulated as to how metal fines or compounds are formed and transferred in the coil and transfer lines exchanger (TLX) of ethylene units. These surface reactions directly or indirectly affect coke formation in the tube. Finally, creep in the coils is likely a factor in promoting corrosion. Such creep is promoted by variable temperature-time patterns to which a coil is exposed during pyrolysis, and then decoking. Periods of stress and compression occur in the coil walls. Knowledge of the diffusion and reactions that take place can result in better furnace operations and decoking procedures to extend the life of the furnace tubes. In this second installment of a four-part series, photomicrographs of four pyrolysis tube samples from the ethylene furnace indicate that significant differences existed between the outer surfaces, inner surfaces, and cross-sectional areas of the samples. The first installment of the series dealt with coke

  2. 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.

  3. Automated, High Temperature Furnace for Glovebox Operation

    International Nuclear Information System (INIS)

    Neikirk, K.

    2001-01-01

    The U.S. Department of Energy will immobilize excess plutonium in the proposed Plutonium Immobilization Plant (PIP) at the Savannah River Site (SRS) as part of a two track approach for the disposition of weapons usable plutonium. As such, the Department of Energy is funding a development and testing effort for the PIP. This effort is being performed jointly by Lawrence Livermore National Laboratory (LLNL), Westinghouse Savannah River Company (WSRC), Pacific Northwest National Laboratory (PNNL), and Argonne National Laboratory (ANL). The Plutonium Immobilization process involves the disposition of excess plutonium by incorporation into ceramic pucks. As part of the immobilization process, furnaces are needed for sintering the ceramic pucks. The furnace being developed for puck sintering is an automated, bottom loaded furnace with insulting package and resistance heating elements located within a nuclear glovebox. Other furnaces considered for the application include retort furnaces and pusher furnaces. This paper, in part, will discuss the furnace technologies considered and furnace technology selected to support reliable puck sintering in a glovebox environment. Due to the radiation levels and contamination associated with the plutonium material, the sintering process will be fully automated and contained within nuclear material gloveboxes. As such, the furnace currently under development incorporates water and air cooling to minimize heat load to the glovebox. This paper will describe the furnace equipment and systems needed to employ a fully automated puck sintering process within nuclear gloveboxes as part of the Plutonium Immobilization Plant

  4. Loss on Ignition Furnace Acceptance and Operability Test Procedure

    International Nuclear Information System (INIS)

    JOHNSTON, D.C.

    2000-01-01

    The purpose of this Acceptance Test Procedure and Operability Test Procedure (ATP/OTP)is to verify the operability of newly installed Loss on Ignition (LOI) equipment, including a model 1608FL CMTM Furnace, a dessicator, and balance. The operability of the furnace will be verified. The arrangement of the equipment placed in Glovebox 157-3/4 to perform LOI testing on samples supplied from the Thermal Stabilization line will be verified. In addition to verifying proper operation of the furnace, this ATP/OTP will also verify the air flow through the filters, verify a damper setting to establish and maintain the required differential pressure between the glovebox and the room pressure, and test the integrity of the newly installed HEPA filter. In order to provide objective evidence of proper performance of the furnace, the furnace must heat 15 crucibles, mounted on a crucible rack, to 1000 C, according to a program entered into the furnace controller located outside the glovebox. The glovebox differential pressure will be set to provide the 0.5 to 2.0 inches of water (gauge) negative pressure inside the glovebox with an expected airflow of 100 to 125 cubic feet per minute (cfm) through the inlet filter. The glovebox inlet G1 filter will be flow tested to ensure the integrity of the filter connections and the efficiency of the filter medium. The newly installed windows and glovebox extension, as well as all disturbed joints, will be sonically tested via ultra probe to verify no leaks are present. The procedure for DOS testing of the filter is found in Appendix A

  5. Loss on Ignition Furnace Acceptance and Operability Test Procedure

    Energy Technology Data Exchange (ETDEWEB)

    JOHNSON, D.C.

    2000-06-01

    The purpose of this Acceptance Test Procedure and Operability Test Procedure (ATP/OTP)is to verify the operability of newly installed LOI equipment, including a model 1608FL CM{trademark} Furnace, a dessicator, and balance. The operability of the furnace will be verified. The arrangement of the equipment placed in Glovebox 157-3/4 to perform Loss on Ignition (LOI) testing on samples supplied from the Thermal Stabilization line will be verified. In addition to verifying proper operation of the furnace, this ATP/OTP will also verify the air flow through the filters, verify a damper setting to establish and maintain the required differential pressure between the glovebox and the room pressure, and test the integrity of the newly installed HEPA filter. In order to provide objective evidence of proper performance of the furnace, the furnace must heat 15 crucibles, mounted on a crucible rack, to 1000 C, according to a program entered into the furnace controller located outside the glovebox. The glovebox differential pressure will be set to provide the 0.5 to 2.0 inches of water (gauge) negative pressure inside the glovebox with an airflow of 100 to 125 cubic feet per minute (cfm) through the inlet filter. The glovebox inlet Glfilter will he flow tested to ensure the integrity of the filter connections and the efficiency of the filter medium. The newly installed windows and glovebox extension, as well as all disturbed joints, will be sonically tested via ultra probe to verify no leaks are present. The procedure for DOS testing of the filter is found in Appendix A.

  6. 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.

  7. Melting temperature of graphite

    International Nuclear Information System (INIS)

    Korobenko, V.N.; Savvatimskiy, A.I.

    2001-01-01

    Full Text: Pulse of electrical current is used for fast heating (∼ 1 μs) of metal and graphite specimens placed in dielectric solid media. Specimen consists of two strips (90 μm in thick) placed together with small gap so they form a black body model. Quasy-monocrystal graphite specimens were used for uniform heating of graphite. Temperature measurements were fulfilled with fast pyrometer and with composite 2-strip black body model up to melting temperature. There were fulfilled experiments with zirconium and tungsten of the same black body construction. Additional temperature measurements of liquid zirconium and liquid tungsten are made. Specific heat capacity (c P ) of liquid zirconium and of liquid tungsten has a common feature in c P diminishing just after melting. It reveals c P diminishing after melting in both cases over the narrow temperature range up to usual values known from steady state measurements. Over the next wide temperature range heat capacity for W (up to 5000 K) and Zr (up to 4100 K) show different dependencies of heat capacity on temperature in liquid state. The experiments confirmed a high quality of 2-strip black body model used for graphite temperature measurements. Melting temperature plateau of tungsten (3690 K) was used for pyrometer calibration area for graphite temperature measurement. As a result, a preliminary value of graphite melting temperature of 4800 K was obtained. (author)

  8. 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

  9. 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.

  10. 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.

  11. Linear expansion of products out of thermal splitting graphite

    International Nuclear Information System (INIS)

    Tishina, E.A.; Kurnevich, G.I.

    1994-01-01

    Linear expansion of thermally split graphite in the form of foil and pressed items of different density was studied. It is ascertained that the extreme character of temperature dependence of linear expansion factor of pressed samples of thermally split graphite is determined by the formation of closed pores containing air in the course of their production. 3 refs., 2 figs

  12. Chemically assisted release of transition metals in graphite vaporizers for atomic spectrometry

    International Nuclear Information System (INIS)

    Katskov, Dmitri; Darangwa, Nicholas; Grotti, Marco

    2006-01-01

    The processes associated with the vaporization of microgram samples and modifiers in a graphite tube ET AAS were investigated by the example of transition metals. The vapor absorption spectra and vaporization behavior of μg-amounts Cd, Zn, Cu, Ag, Au, Ni, Co, Fe, Mn and Cr were studied using the UV spectrometer with CCD detector, coupled with a continuum radiation source. The pyrocoated, Ta or W lined tubes, with Ar or He as internal gases, and filter furnace were employed in the comparative experiments. It was found that the kinetics of atomic vapor release changed depending on the specific metal-substrate-gas combination; fast vaporization at the beginning was followed by slower 'tailing.' The absorption continuum, overlapped by black body radiation at longer wavelengths, accompanied the fast vaporization mode for all metals, except Cd and Zn. The highest intensity of the continuum was observed in the pyrocoated tube with Ar. For Cu and Ag the molecular bands overlapped the absorption continuum; the continuum and bands were suppressed in the filter furnace. It is concluded that the exothermal interaction of sample vapor with the material of the tube causes the energy evolution in the gas phase. The emitted heat is dispersed near the tube wall in the protective gas and partially transferred back to the surface of the sample, thus facilitating the vaporization. The increased vapor flow causes over-saturation and gas-phase condensation in the absorption volume at some distance from the wall, where the gas temperature is not affected by the reaction. The condensation is accompanied by the release of phase transition energy via black body radiation and atomic emission. The particles of condensate and molecular clusters cause the scattering of light and molecular absorption; slow decomposition of the products of the sample vapor-substrate reaction produces the 'tailing' of atomic absorption signal. The interaction of graphite with metal vapor or oxygen, formed in the

  13. Dislocation density and graphitization of diamond crystals

    International Nuclear Information System (INIS)

    Pantea, C.; Voronin, G.A.; Zerda, T.W.; Gubicza, J.; Ungar, T.

    2002-01-01

    Two sets of diamond specimens compressed at 2 GPa at temperatures varying between 1060 K and 1760 K were prepared; one in which graphitization was promoted by the presence of water and another in which graphitization of diamond was practically absent. X-ray diffraction peak profiles of both sets were analyzed for the microstructure by using the modified Williamson-Hall method and by fitting the Fourier coefficients of the measured profiles by theoretical functions for crystallite size and lattice strain. The procedures determined mean size and size distribution of crystallites as well as the density and the character of the dislocations. The same experimental conditions resulted in different microstructures for the two sets of samples. They were explained in terms of hydrostatic conditions present in the graphitized samples

  14. Reactivity of lithium exposed graphite surface

    International Nuclear Information System (INIS)

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

    2009-01-01

    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.

  15. Sensing capabilities of graphite based MR elastomers

    International Nuclear Information System (INIS)

    Tian, T F; Li, W H; Deng, Y M

    2011-01-01

    This paper presents both experimental and theoretical investigations of the sensing capabilities of graphite based magnetorheological elastomers (MREs). In this study, eight MRE samples with varying graphite weight fractions were fabricated and their resistance under different magnetic fields and external loadings were measured with a multi-meter. With an increment of graphite weight fraction, the resistance of MRE sample decreases steadily. Higher magnetic fields result in a resistance increase. Based on an ideal assumption of a perfect chain structure, a mathematical model was developed to investigate the relationship between the MRE resistance with external loading. In this model, the current flowing through the chain structure consists of both a tunnel current and a conductivity current, both of which depend on external loadings. The modelling parameters have been identified and reconstructed from comparison with experimental results. The comparison indicates that both experimental results and modelling predictions agree favourably well

  16. Nuclear graphite ageing and turnaround

    International Nuclear Information System (INIS)

    Marsden, B.J.; Hall, G.N.; Smart, J.

    2001-01-01

    Graphite moderated reactors are being operated in many countries including, the UK, Russia, Lithuania, Ukraine and Japan. Many of these reactors will operate well into the next century. New designs of High Temperature Graphite Moderated Reactors (HTRS) are being built in China and Japan. The design life of these graphite-moderated reactors is governed by the ageing of the graphite core due to fast neutron damage, and also, in the case of carbon dioxide cooled reactors by the rate of oxidation of the graphite. Nuclear graphites are polycrystalline in nature and it is the irradiation-induced damage to the individual graphite crystals that determines the material property changes with age. The life of a graphite component in a nuclear reactor can be related to the graphite irradiation induced dimensional changes. Graphites typically shrink with age, until a point is reached where the shrinkage stops and the graphite starts to swell. This change from shrinkage to swelling is known as ''turnaround''. It is well known that pre-oxidising graphite specimens caused ''turnaround'' to be delayed, thus extending the life of the graphite, and hence the life of the reactor. However, there was no satisfactory explanation of this behaviour. This paper presents a numerical crystal based model of dimensional change in graphite, which explains the delay in ''turnaround'' in the pre-oxidised specimens irradiated in a fast neutron flux, in terms of crystal accommodation and orientation and change in compliance due to radiolytic oxidation. (author)

  17. Materials analyses of ceramics for glass furnace recuperators

    Energy Technology Data Exchange (ETDEWEB)

    Weber, G.W.; Tennery, V.J.

    1979-11-01

    The use of waste heat recuperation systems offers significant promise for meaningful energy conservation in the process heat industries. This report details the analysis of candidate ceramic recuperator materials exposed to simulated industrial glass furnace hot flue gas environments. Several candidate structural ceramic materials including various types of silicon carbide, several grades of alumina, mullite, cordierite, and silicon nitride were exposed to high-temperature flue gas atmospheres from specially constructed day tank furnaces. Furnace charging, operation, and batch composition were selected to closely simulate industrial practice. Material samples were exposed in flues both with and without glass batch in the furnace for times up to 116 d at temperatures from 1150 to 1550/sup 0/C (2100 to 2800/sup 0/F). Exposed materials were examined by optical microscopy, scanning electron microscopy, energy dispersive x-ray analysis, x-ray diffraction, and x-ray fluorescence to identify material degradation mechanisms. The materials observations were summarized as: Silicon carbide exhibited enhanced corrosion at lower temperatures (1150/sup 0/C) when alkalies were deposited on the carbide from the flue gas and less corrosion at higher temperatures (1550/sup 0/C) when alkalies were not deposited on the carbide; alumina corrosion depended strongly upon purity and density and alumina contents less than 99.8% were unsatisfactory above 1400/sup 0/C; and mullite and cordierite are generally unacceptable for application in soda-lime glass melting environments at temperatures above 1100/sup 0/C.

  18. 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.

  19. Preparation of graphite targets for radiocarbon dating by tandem accelerator mass spectrometer (TAMS)

    International Nuclear Information System (INIS)

    Lowe, D.C.

    1984-01-01

    The introduction of TAMS has exciting implications for radiocarbon dating but improved sample preparation methods are needed. This paper describes a promising method for the conversion of a few milligrams of wood or charcoal into graphite targets for use in a caesium sputter ion source. Targets containing a large proportion of G-type graphite produced large C - currents, but those containing a high proportion of turbostatic Tn graphite were unsatisfactory; the type of graphite in the target is clearly of significance. (author)

  20. Bromine intercalated graphite for lightweight composite conductors

    KAUST Repository

    Amassian, Aram; Patole, Archana

    2017-01-01

    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

  1. Cesium diffusion in graphite

    International Nuclear Information System (INIS)

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

    1980-05-01

    Experiments on diffusion of 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 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 0 C in a helium atmosphere is essentially pure diffusion wherein values of (E/epsilon) and ΔE of the equation D/epsilon = (D/epsilon) 0 exp [-ΔE/RT] are about 4 x 10 -2 cm 2 /s and 30 kcal/mole, respectively

  2. Fluorophotometric determination of uranium: an automated sintering furnace and factors affecting precision

    International Nuclear Information System (INIS)

    Strain, J.E.

    1978-07-01

    The fusion furnace consists of four individually controlled, slotted-tube furnaces that automatically dry, sinter and anneal the fluoride or carbonate pellet used in the fluorometric determination of uranium. The furnace operates in air and prepares approximately 90 pellets per hour for fluorometric measurement. The factors that were thought to affect the precision of the method were investigated. The two factors that seem to be the most influential are (1) the manner in which the sample is loaded onto the pellet; and (2) the surface characteristics of the platinum dish in which the pellet is sintered and measured fluorometrically

  3. Refractory of Furnaces to Reduce Environmental Impact

    Science.gov (United States)

    Hanzawa, Shigeru

    2011-10-01

    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 CO2 produced from this high energy load. To improve this situation, R&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-CO2 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.

  4. Fluxless furnace brazing and its theoretical fundamentals

    International Nuclear Information System (INIS)

    Lison, R.

    1979-01-01

    In this paper the theoretical fundamental of fluxless furnace brazing are described. The necessary conditions for a wetting in the vacuum, under a inert-gas and with a reducing gas are discussed. Also other methods to reduce the oxygen partial pressure are described. Some applications of fluxless furnace brazing are outlined. (orig.) [de

  5. Refractory of Furnaces to Reduce Environmental Impact

    International Nuclear Information System (INIS)

    Hanzawa, Shigeru

    2011-01-01

    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 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 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.

  6. The use of blast furnace slag

    Directory of Open Access Journals (Sweden)

    V. Václavík

    2012-10-01

    Full Text Available The paper presents the results of experimental research that dealt with the substitution of finely ground blast furnace slag for Portland cement in the course of simple concrete manufacturing. Physical and mechanical properties of experimental concrete mixtures based on finely ground blast furnace slag were observed.

  7. Direct reading spectrochemical analysis of nuclear graphite

    International Nuclear Information System (INIS)

    Roca Adell, M.; Becerro Ruiz, E.; Alvarez Gonzalez, F.

    1964-01-01

    A description is given about the application of a direct-reading spectrometer the Quantometer, to the determination of boron. calcium, iron, titanium and vanadium in nuclear grade graphite. for boron the powdered sample is mixed with 1% cupric fluoride and excited in a 10-amperes direct current arc and graphite electrodes with a crater 7 mm wide and 10 mm deep. For the other elements a smaller crater has been used and dilution with a number of matrices has been investigated; the best results are achieved by employing 25% cupric fluoride. The sensitivity limit for boron is 0,15 ppm. (Author) 21 refs

  8. Irradiation-induced amorphization process in graphite

    Energy Technology Data Exchange (ETDEWEB)

    Abe, Hiroaki [Japan Atomic Energy Research Inst., Takasaki, Gunma (Japan). Takasaki Radiation Chemistry Research Establishment

    1996-04-01

    Effects of the element process of irradiation damage on irradiation-induced amorphization processes of graphite was studied. High orientation thermal decomposed graphite was cut about 100 nm width and used as samples. The irradiation experiments are carried out under the conditions of electronic energy of 100-400 KeV, ion energy of 200-600 KeV, ionic species Xe, Ar, Ne, C and He and the irradiation temperature at from room temperature to 900 K. The critical dose ({phi}a) increases exponentially with increasing irradiation temperature. The displacement threshold energy of graphite on c-axis direction was 27 eV and {phi}a{sup e} = 0.5 dpa. dpa is the average number of displacement to atom. The critical dose of ion irradiation ({phi}a{sup i}) was 0.2 dpa at room temperature, and amorphous graphite was produced by less than half of dose of electronic irradiation. Amorphization of graphite depending upon temperature is discussed. (S.Y.)

  9. Intercomparison of graphite irradiations

    Energy Technology Data Exchange (ETDEWEB)

    Hering, H; Perio, P; Seguin, M [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1959-07-01

    While fast neutrons only are effective in damaging graphite, results of irradiations are more or less universally expressed in terms of thermal neutron fluxes. This paper attempts to correlate irradiations made in different reactors, i.e., in fluxes of different spectral compositions. Those attempts are based on comparison of 1) bulk length change and volume expansion, and 2) crystalline properties (e.g., lattice parameter C, magnetic susceptibility, stored energy, etc.). The methods used by various authors for determining the lattice constants of irradiated graphite are discussed. (author)

  10. Optical cavity furnace for semiconductor wafer processing

    Science.gov (United States)

    Sopori, Bhushan L.

    2014-08-05

    An optical cavity furnace 10 having multiple optical energy sources 12 associated with an optical cavity 18 of the furnace. The multiple optical energy sources 12 may be lamps or other devices suitable for producing an appropriate level of optical energy. The optical cavity furnace 10 may also include one or more reflectors 14 and one or more walls 16 associated with the optical energy sources 12 such that the reflectors 14 and walls 16 define the optical cavity 18. The walls 16 may have any desired configuration or shape to enhance operation of the furnace as an optical cavity 18. The optical energy sources 12 may be positioned at any location with respect to the reflectors 14 and walls defining the optical cavity. The optical cavity furnace 10 may further include a semiconductor wafer transport system 22 for transporting one or more semiconductor wafers 20 through the optical cavity.

  11. 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...... 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...... 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....

  12. Graphite fiber/copper composites prepared by spontaneous infiltration

    Science.gov (United States)

    Wang, Hongbao; Tao, Zechao; Li, Xiangfen; Yan, Xi; Liu, Zhanjun; Guo, Quangui

    2018-05-01

    The major bottleneck in developing graphite fiber reinforced copper (GF/Cu) composites is the poor wettability of Cu/graphite system. Alloying element of chromium (Cr) is introduced to improve the wettability of liquid copper on graphite. Sessile drop method experiments illustrate that the contact angle of liquid Cu-Cr (1.0 wt.%) alloy on graphite substrate decreases to 43° at 1300 °C. The improvement of wettability is related to the formation of chromium carbide layer at interface zone. Based on the wetting experiment, a spontaneous infiltration method for preparing GF/Cu composites is proposed. Unidirectional GF preforms are infiltrated by Cu-Cr alloys without external pressure in a tubular furnace. Results reveal that the GF preform can be fully infiltrated by Cu-Cr alloy (8 wt.%) spontaneously when fiber volume fraction is 40%. The coefficient of thermal expansion (CTE) of GF/Cu-Cr (8.0 wt.%) composites is 4.68 × 10-6/K along the longitudinal direction.

  13. Comparison of Oxidation Characteristics of Selected Nuclear Graphite Grades

    International Nuclear Information System (INIS)

    Chi, Se Hwan; Kim, Gen Chan

    2010-02-01

    The oxidation behavior of some selected nuclear graphite grades (i.e., IG-110, IG-430, NBG-18, NBG-25) were compared in view of their filler coke type and the physical property of the grades. Oxidation rates were determined at six temperatures between 600 ∼ 960 .deg. C in air by using a three-zone vertical tube furnace at a 10 L/min air flow rate. The specimens were a cylinder with a 25.4 mm diameter and a 25.4 mm length. Results showed that, even though the four examined nuclear graphite grades showed a highly temperature-sensitive oxidation behavior through out the test temperature range of 600 ∼ 950 .deg. C, the differences between the grades were not significant. The oxidation rates determined for a 5∼10 % weight loss at the six temperatures were nearly the same except for 702 and 808 .deg. C, where the pitch coke graphites showed an apparent decrease in their oxidation rate, more so than the petroleum coke graphites. These effects of the coke type reduced or nearly disappeared with an increasing temperature. The average activation energy determined for 608 ∼ 808 .deg. C was 161.5 ± 7.3 kJ/mol, showing that the dominant oxidation reaction occurred by a chemical control

  14. 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.

  15. Biomass furnace: projection and construction

    Energy Technology Data Exchange (ETDEWEB)

    Melo, Fernanda Augusta de Oliveira; Silva, Juarez Sousa e; Silva, Denise de Freitas; Sampaio, Cristiane Pires; Nascimento Junior, Jose Henrique do [Universidade Federal de Vicosa (DEA/UFV), MG (Brazil). Dept. de Engenharia Agricola

    2008-07-01

    Of all the ways to convert biomass into thermal energy, direct combustion is the oldest. The thermal-chemical technologies of biomass conversion such as pyrolysis and gasification, are currently not the most important alternatives; combustion is responsible for 97% of the bio-energy produced in the world (Demirbas, 2003). For this work, a small furnace was designed and constructed to use biomass as its main source of fuel, and the combustion chamber was coupled with a helical transporter which linked to the secondary fuel reservoir to continually feed the combustion chamber with fine particles of agro-industrial residues. The design of the stove proved to be technically viable beginning with the balance of mass and energy for the air heating system. The proposed heat generator was easily constructed as it made use of simple and easily acquired materials, demanding no specialized labor. (author)

  16. Glassy carbon coated graphite for nuclear applications

    International Nuclear Information System (INIS)

    Delpeux S; Cacciaguerra T; Duclaux L

    2005-01-01

    Taking into account the problems caused by the treatment of nuclear wastes, the molten salts breeder reactors are expected to a great development. They use a molten fluorinated salt (mixture of LiF, BeF 2 , ThF 4 , and UF 4 ) as fuel and coolant. The reactor core, made of graphite, is used as a neutrons moderator. Despite of its compatibility with nuclear environment, it appears crucial to improve the stability and inertness of graphite against the diffusion of chemicals species leading to its corrosion. One way is to cover the graphite surface by a protective impermeable deposit made of glassy carbon obtained by the pyrolysis of phenolic resin or polyvinyl chloride precursors. The main difficulty in the synthesis of glassy carbon is to create exclusively, in the primary pyrolysis product, a micro-porosity of about twenty Angstroms which closes later at higher temperature. Therefore, the evacuation of the volatile products occurring mainly between 330 and 600 C, must progress slowly to avoid the material to crack. In this study, the optimal parameters for the synthesis of glassy carbon as well as glassy carbon deposits on nuclear-type graphite pieces are discussed. Both thermal treatment of phenolic and PVC resins have been performed. The structure and micro-texture of glassy carbon have been investigated by X-ray diffraction, scanning and transmission electron microscopies and helium pycno-metry. Glassy carbon samples (obtained at 1200 C) show densities ranging from 1.3 to 1.55 g/cm 3 and closed pores with nano-metric size (∼ 5 to 10 nm) appear clearly on the TEM micrographs. Then, a thermal treatment to 2700 C leads to the shrinkage of the entangled graphene ribbons, in good agreement with the proposed texture model for glassy carbon. Glassy carbon deposits on nuclear graphite have been developed by an impregnation method. The uniformity of the deposit depends clearly on the surface texture and the chemistry of the graphite substrate. The deposit regions where

  17. Glassy carbon coated graphite for nuclear applications

    Energy Technology Data Exchange (ETDEWEB)

    Delpeux, S.; Cacciaguerra, T.; Duclaux, L. [Orleans Univ., CRMD, CNRS, 45 (France)

    2005-07-01

    Taking into account the problems caused by the treatment of nuclear wastes, the molten salts breeder reactors are expected to a great development. They use a molten fluorinated salt (mixture of LiF, BeF{sub 2}, ThF{sub 4}, and UF{sub 4}) as fuel and coolant. The reactor core, made of graphite, is used as a neutrons moderator. Despite of its compatibility with nuclear environment, it appears crucial to improve the stability and inertness of graphite against the diffusion of chemicals species leading to its corrosion. One way is to cover the graphite surface by a protective impermeable deposit made of glassy carbon obtained by the pyrolysis of phenolic resin [1,2] or polyvinyl chloride [3] precursors. The main difficulty in the synthesis of glassy carbon is to create exclusively, in the primary pyrolysis product, a micro-porosity of about twenty Angstroms which closes later at higher temperature. Therefore, the evacuation of the volatile products occurring mainly between 330 and 600 C, must progress slowly to avoid the material to crack. In this study, the optimal parameters for the synthesis of glassy carbon as well as glassy carbon deposits on nuclear-type graphite pieces are discussed. Both thermal treatment of phenolic and PVC resins have been performed. The structure and micro-texture of glassy carbon have been investigated by X-ray diffraction, scanning and transmission electron microscopies and helium pycno-metry. Glassy carbon samples (obtained at 1200 C) show densities ranging from 1.3 to 1.55 g/cm{sup 3} and closed pores with nano-metric size ({approx} 5 to 10 nm) appear clearly on the TEM micrographs. Then, a thermal treatment to 2700 C leads to the shrinkage of the entangled graphene ribbons (Fig 1), in good agreement with the proposed texture model for glassy carbon (Fig 2) [4]. Glassy carbon deposits on nuclear graphite have been developed by an impregnation method. The uniformity of the deposit depends clearly on the surface texture and the chemistry

  18. Production technique of vermicular graphite iron cylinder head of vehicle diesel engine

    Directory of Open Access Journals (Sweden)

    Zhou Gen

    2008-11-01

    Full Text Available The 25 years’production and application have proved that vermicular graphite iron cylinder heads with vermicularity ≥50% satisfy the machinability and performance demand of diesel engine. The method, in which using cupola-induction furnace duplex melting and pour-over process with rare earth-ferrosilicon or rare earthsilicon compound as vermicularizing alloy plus rare earth-magnesium-ferrosilicon as stirring alloy, is an optimal vermicularizing process for obtaining satisfi ed vermicularity. Using top kiss risers, enlarging kissing areas and expanding covering width and making ingates to freeze earlier are the effective measures to eliminate shrinkage, blowhole and oxide inclusions in the vermicular graphite iron cylinder heads.

  19. Ion irradiation to simulate neutron irradiation in model graphites: Consequences for nuclear graphite

    Science.gov (United States)

    Galy, N.; Toulhoat, N.; Moncoffre, N.; Pipon, Y.; Bérerd, N.; Ammar, M. R.; Simon, P.; Deldicque, D.; Sainsot, P.

    2017-10-01

    Due to its excellent moderator and reflector qualities, graphite was used in CO2-cooled nuclear reactors such as UNGG (Uranium Naturel-Graphite-Gaz). Neutron irradiation of graphite resulted in the production of 14C which is a key issue radionuclide for the management of the irradiated graphite waste. In order to elucidate the impact of neutron irradiation on 14C behavior, we carried out a systematic investigation of irradiation and its synergistic effects with temperature in Highly Oriented Pyrolitic Graphite (HOPG) model graphite used to simulate the coke grains of nuclear graphite. We used 13C implantation in order to simulate 14C displaced from its original structural site through recoil. The collision of the impinging neutrons with the graphite matrix carbon atoms induces mainly ballistic damage. However, a part of the recoil carbon atom energy is also transferred to the graphite lattice through electronic excitation. The effects of the different irradiation regimes in synergy with temperature were simulated using ion irradiation by varying Sn(nuclear)/Se(electronic) stopping power. Thus, the samples were irradiated with different ions of different energies. The structure modifications were followed by High Resolution Transmission Electron Microscopy (HRTEM) and Raman microspectrometry. The results show that temperature generally counteracts the disordering effects of irradiation but the achieved reordering level strongly depends on the initial structural state of the graphite matrix. Thus, extrapolating to reactor conditions, for an initially highly disordered structure, irradiation at reactor temperatures (200 - 500 °C) should induce almost no change of the initial structure. On the contrary, when the structure is initially less disordered, there should be a "zoning" of the reordering: In "cold" high flux irradiated zones where the ballistic damage is important, the structure should be poorly reordered; In "hot" low flux irradiated zones where the ballistic

  20. Automated handling for SAF batch furnace and chemistry analysis operations

    International Nuclear Information System (INIS)

    Bowen, W.W.; Sherrell, D.L.; Wiemers, M.J.

    1981-01-01

    The Secure Automated Fabrication Program is developing a remotely operated breeder reactor fuel pin fabrication line. The equipment will be installed in the Fuels and Materials Examination Facility being constructed at Hanford, Washington. Production is scheduled to start in mid-1986. The application of small pneumatically operated industrial robots for loading and unloading product into and out of batch furnaces and for distribution and handling of chemistry samples is described

  1. [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.

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

    Directory of Open Access Journals (Sweden)

    E. A. Pitukhin

    2016-03-01

    Full Text Available 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 chamber up to 1250ºC. Fire-resistance limit for the test samples of composite material is determined by the loss of insulating ability (I. For that purpose, the time is obtained from the test beginning with the standard temperature mode up to a limiting condition. Main Results. In accordance with the requirements of regulatory documents fire-resistance limit I15 has been obtained equal to 15 minutes. The qualitative and quantitative phase analysis of the CM structure has been done. By the study of samples by X-ray diffraction and electron microscopy we have determined that the material retains the same chemical structure with a monotonic heating above 700° C. Practical Relevance. The composite material with obtained characteristics can be used as a protective coating for building constructions with the aim of fire-resistance enhancement and fuel hazard reduction.

  3. The movement of the burden in submerged-arc furnaces for the production of high-carbon ferromanganese

    International Nuclear Information System (INIS)

    Dyason, G.J.; See, J.B.

    1978-01-01

    The mechanism by which the burden moves in a submerged-arc furnace was investigated in two large industrial furnaces by the stimulus-response technique with a radiotracer of the radio-isotope 5 Fe as the stimulus. As this radio-isotope was suitable only for the measurement of residence-time distributions in the alloy phase, the analysis of the experiments was limited to that phase. The residence-time distributions obtained by the measurement of alloy samples obtained during tapping were analysed by various techniques. This analysis verified the existence of stagnant zones within the furnace, and showed that the movement of the burden through the furnace could not be described by either of the two idealized patterns of flow, i.e., plug flow or mixed flow. A composite model to describe the movement of the burden through the furnace was developed by consideration of the mechanism and position of heat generation within the furnace, the inner structure of the furnace, the general form of the measured residence-time distributions, and the mode of burden descent through the furnace. The composite model consisted of a dispersed plug-flow region in the upper regions of the furnace discharging into a constantly stirred tank reactor beneath the electrode tips. Non-linear regression analysis of the equations developed from the composite model permitted the selection of optimum values of model parameters to give computed curves that approximated to the residence-time distributions [af

  4. Determination of chlorine in graphite by combustion-ion chromatography

    International Nuclear Information System (INIS)

    Chen Lianzhong; Watanabe, Kazuo; Itoh, Mitsuo.

    1995-09-01

    A combustion/ion chromatographic method has been studied for the sensitive determination of chlorine in graphite. A graphite sample was burnt at 900degC in a silica reaction tube at an oxygen flow rate of 200 ml/min. Chlorine evolved was absorbed in 20 ml of a 0.1 mM sodium carbonate solution. The solution was evaporated to dryness. The residue was dissolved with a small volume of water. Chlorine in the solution was determined using ion chromatography. The method was applied to JAERI graphite certified reference materials and practical graphite materials. The detection limit was about 0.8 μgCl/g for a 2.0 g sample. The precision was about 2.5% (relative standard deviation) for samples with chlorine content of 70 μg/g level. The method is also usable for coal samples. (author)

  5. A study on the formation of uranium carbide in an induction furnace

    International Nuclear Information System (INIS)

    Song, In Young; Lee, Yoon Sang; Kim, Eung Soo; Lee, Don Bae; Kim, Chang Kyu

    2005-01-01

    Uranium is a typical carbide-forming element. Three carbides, UC, U 2 C 3 and UC 2 , are formed in the uranium-carbon system. The most important of these as fuel is uranium monocarbide UC. It is well known that Uranium carbides can be obtained by three basic methods: 1) by reaction of uranium metal with carbon; 2) by reaction of uranium metal powder with gaseous hydrocarbons; 3) by reaction of uranium oxides with carbon. The use of uranium monocarbide, or materials based on it, has great prospects as fuel for nuclear reactors. It is quite possible that uranium dicarbide UC 2 may also acquire great importance as a fuel, particularly in dispersion fuel elements with graphite matrix. In the present study, uranium carbides are obtained by direct reaction of uranium metal with graphite in a high frequency induction furnace

  6. Uranium casting furnace automatic temperature control development

    International Nuclear Information System (INIS)

    Lind, R.F.

    1992-01-01

    Development of an automatic molten uranium temperature control system for use on batch-type induction casting furnaces is described. Implementation of a two-color optical pyrometer, development of an optical scanner for the pyrometer, determination of furnace thermal dynamics, and design of control systems are addressed. The optical scanning system is shown to greatly improve pyrometer measurement repeatability, particularly where heavy floating slag accumulations cause surface temperature gradients. Thermal dynamics of the furnaces were determined by applying least-squares system identification techniques to actual production data. A unity feedback control system utilizing a proportional-integral-derivative compensator is designed by using frequency-domain techniques. 14 refs

  7. Programmable temperature regulator of VAO-1 furnace

    International Nuclear Information System (INIS)

    Zahalka, F.

    1979-01-01

    A programmable temperature controller is described for a furnace for high-level waste processing. Furnace temperature is controlled by a program compiled from a combination of 3 parts with different linear increments or decrements of time dependent temperature and 2 parts with isothermal control for over a preset period. The equipment consists essentially of a programming unit, a programmed digital-to-analog converter and a power unit. The design is described in detail and its specifications are given. The maximum operating temperature of 1500 degC may be reached in the furnace charge section. (B.S.)

  8. Alternative fuels for multiple-hearth furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Bracket, B D; Lawson, T U

    1980-04-01

    Results are described of a feasibility study on the use of refuse-derived fuel, shredded paper, wood waste, coal, and waste oil in multiple-hearth furnaces at the Lower Molonglo Water Quality Control Centre in Australia. An assessment of waste fuel availability and characteristics is given, and a summary is made of the technical and economic aspects of using these alternative fuels and of minimizing furnace fuel requirements by reducing sludge moisture. The recommended method of reducing fuel oil consumption in the furnace is shown to be sludge drying, using process exhaust heat in a rotary dryer.

  9. Internal heat exchange tubes for industrial furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Hoetzl, M.; Lingle, T.M.

    1992-05-26

    This patent describes a method for cooling the work within an industrial furnace. It comprises providing a longitudinally extending outer tube which extends into the furnace having a closed axial end and an open axial end; providing a preformed inner tube open at both ends within the outer tube; injecting a coolant into the inner tube so that the coolant flows from one axial end of the tube out the opposite end adjacent the closed end of the outer tube, and from the closed end of the outer tube to the open end thereof; circulating a gas within the furnace against the outer tube to effect heat transfer therewith.

  10. Production technique of vermicular graphite iron cylinder head of vehicle diesel engine

    OpenAIRE

    Zhou Gen; Liu Wanhua

    2008-01-01

    The 25 years’production and application have proved that vermicular graphite iron cylinder heads with vermicularity ≥50% satisfy the machinability and performance demand of diesel engine. The method, in which using cupola-induction furnace duplex melting and pour-over process with rare earth-ferrosilicon or rare earthsilicon compound as vermicularizing alloy plus rare earth-magnesium-ferrosilicon as stirring alloy, is an optimal vermicularizing process for obtaining satisfi ed vermicularity. ...

  11. Magnetic orientation of paraffin in a magnetic levitation furnace

    Science.gov (United States)

    Takahashi, K.; Umeki, C.; Mogi, I.; Koyama, K.; Awaji, S.; Motokawa, M.; Watanabe, K.

    2004-04-01

    Containerless melting of paraffin under a magnetic levitation condition has been performed by using a cryogen-free hybrid magnet and two kinds of laser furnaces. One is local irradiation of CO 2 laser light at the top of the sample. The other is homogeneous irradiation of YAG laser light with a concave ring mirror. In the latter case, reduction of the Marangoni convection on the surface of the sample and the magnetic orientation of paraffin molecules were observed. The magnetic anisotropy of the spherical sample was confirmed by the measurement of magnetization and X-ray diffraction.

  12. Magnetic orientation of paraffin in a magnetic levitation furnace

    Energy Technology Data Exchange (ETDEWEB)

    Takahashi, K.; Umeki, C.; Mogi, I.; Koyama, K.; Awaji, S.; Motokawa, M.; Watanabe, K

    2004-04-30

    Containerless melting of paraffin under a magnetic levitation condition has been performed by using a cryogen-free hybrid magnet and two kinds of laser furnaces. One is local irradiation of CO{sub 2} laser light at the top of the sample. The other is homogeneous irradiation of YAG laser light with a concave ring mirror. In the latter case, reduction of the Marangoni convection on the surface of the sample and the magnetic orientation of paraffin molecules were observed. The magnetic anisotropy of the spherical sample was confirmed by the measurement of magnetization and X-ray diffraction.

  13. Magnetic orientation of paraffin in a magnetic levitation furnace

    International Nuclear Information System (INIS)

    Takahashi, K.; Umeki, C.; Mogi, I.; Koyama, K.; Awaji, S.; Motokawa, M.; Watanabe, K.

    2004-01-01

    Containerless melting of paraffin under a magnetic levitation condition has been performed by using a cryogen-free hybrid magnet and two kinds of laser furnaces. One is local irradiation of CO 2 laser light at the top of the sample. The other is homogeneous irradiation of YAG laser light with a concave ring mirror. In the latter case, reduction of the Marangoni convection on the surface of the sample and the magnetic orientation of paraffin molecules were observed. The magnetic anisotropy of the spherical sample was confirmed by the measurement of magnetization and X-ray diffraction

  14. 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.

  15. 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.

  16. System design description for the whole element furnace testing system

    International Nuclear Information System (INIS)

    Ritter, G.A.; Marschman, S.C.; MacFarlan, P.J.; King, D.A.

    1998-05-01

    This document provides a detailed description of the Hanford Spent Nuclear Fuel (SNF) Whole Element Furnace Testing System located in the Postirradiation Testing Laboratory G-Cell (327 Building). Equipment specifications, system schematics, general operating modes, maintenance and calibration requirements, and other supporting information are provided in this document. This system was developed for performing cold vacuum drying and hot vacuum drying testing of whole N-Reactor fuel elements, which were sampled from the 105-K East and K West Basins. The proposed drying processes are intended to allow dry storage of the SNF for long periods of time. The furnace testing system is used to evaluate these processes by simulating drying sequences with a single fuel element and measuring key system parameters such as internal pressures, temperatures, moisture levels, and off-gas composition

  17. Graphite electrode dc arc technology development for treatment of buried wastes

    International Nuclear Information System (INIS)

    Surma, J.E.; Cohn, D.R.; Smatlak, D.L.; Thomas, P.; Woskov, P.P.

    1993-02-01

    A ''National Laboratory-University-Industrial'' three-way partnership has been established between the Pacific Northwest Laboratory (PNL), Massachusetts Institute of Technology (MIT), and Electro-Pyrolysis, Inc. (EPI) to develop graphite electrode DC arc technology for the treatment of buried wastes. This paper outlines the PNL-MIT-EPI program describing a series of engineering-scale DC arc furnace tests conducted in an EPI furnace at the Plasma Fusion Center at MIT, and a description of the second phase of this program involving the design, fabrication, and testing of a pilot-scale DC arc furnace. Included in this work is the development and implementation of diagnostics to evaluate and optimize high temperature thermal processes such as the DC arc technology

  18. A high resolution electron microscopy investigation of curvature in multilayer graphite sheets

    International Nuclear Information System (INIS)

    Wang Zhenxia; Hu Jun; Wang Wenmin; Yu Guoqing

    1998-01-01

    Here the authors report a carbon sample generated by ultrasonic wave high oriented pyrolytic graphite (HOPG) in ethanol, water or ethanol-water mixed solution. High resolution transmission electron microscopy (HRTEM) revealed many multilayer graphite sheets with a total curved angle that is multiples of θ 0 (= 30 degree C). Close examination of the micrographs showed that the curvature is accomplished by bending the lattice planes. A possible explanation for the curvature in multilayer graphite sheets is discussed based on the conformation of graphite symmetry axes and the formation of sp 3 -like line defects in the sp 2 graphitic network

  19. 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.

  20. International blast furnace hearth and raceway symposium

    Energy Technology Data Exchange (ETDEWEB)

    1981-01-01

    Papers presented discussed some of the physical and chemical processes occuring in the raceway and hearths of blast furnaces. The injection of coal or fuel slurries to replace some of the coke was also covered. Fourteen papers are abstracted separately.

  1. Multiple hearth furnace for reducing iron oxide

    Science.gov (United States)

    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).

  2. Hopewell Furnace NHS : alternative transportation study

    Science.gov (United States)

    2009-12-31

    This study assesses the potential for an alternative transportation system (ATS) at Hopewell Furnace National Historic Site (NHS). The Volpe Center investigated internal circulation and potential partnerships with local historic, cultural, and recrea...

  3. Metallurgy of mercury in Almaden: from aludel furnaces until Pacific furnaces

    International Nuclear Information System (INIS)

    Tejero-Manzanares, J.; Garrido Saenz, I.; Mata Cabrera, F.; Rubio Mesas, M. L.

    2014-01-01

    This paper shows the different types of furnaces for roasting cinnabar, used in the metallurgy of quicksilver over the centuries of exploitation of the Almaden Mines (Spain). Some of these techniques are part of our industrial heritage. They have contributed to name UNESCO World Heritage Site the vast technological legacy of these mines recently. This research contributes to close the long way of metallurgical activity from aludel furnaces until Pacif furnaces, first and lasted technology to produce on an industrial scale. It is delved into the most relevant aspects having to do with the type, evolution and number of furnaces existing on each of the periods. (Author)

  4. A furnace for firing carbon products

    Energy Technology Data Exchange (ETDEWEB)

    Sudavskii, A M

    1979-12-05

    A furnace for firing carbon products is patented that consists of several chambers with a perforated hearth, which are interconnected by a lower and an upper reservoir with a locking fixture, and a flue. In order to intensify the firing process by increasing the specific hearth productivity, the flue is connected to the upper reservoir. A block diagram of the patented furnace is given, together with a description of its operation.

  5. 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.

  6. Multiphase flow modelling of furnace tapholes

    OpenAIRE

    Reynolds, Quinn G.; Erwee, Markus W.

    2017-01-01

    Pyrometallurgical furnaces of many varieties make use of tapholes in order to facilitate the removal of molten process material from inside the vessel. Correct understanding and operation of the taphole is essential for optimal performance of such furnaces. The present work makes use of computational fluid dynamics models generated using the OpenFOAM® framework in order to study flow behaviour in the taphole system. Single-phase large-eddy simulation models are used to quantify the discharge ...

  7. A standard graphite block

    Energy Technology Data Exchange (ETDEWEB)

    Ivkovic, M; Zdravkovic, Z; Sotic, O [Department of Reactor Physics and Dynamics, Boris Kidric Institute of nuclear sciences Vinca, Belgrade (Yugoslavia)

    1966-04-15

    A graphite block was calibrated for the thermal neutron flux of the Ra-Be source using indium foils as detectors. Experimental values of the thermal neutron flux along the central vertical axis of the system were corrected for the self-shielding effect and depression of flux in the detector. The experimental values obtained were compared with the values calculated on the basis of solving the conservation neutron equation by the continuous slowing-down theory. In this theoretical calculation of the flux the Ra-Be source was divided into three resonance energy regions. The measurement of the thermal neutron diffusion length in the standard graphite block is described. The measurements were performed in the thermal neutron region of the system. The experimental results were interpreted by the diffusion theory for point thermal neutron source in the finite system. The thermal neutron diffusion length was calculated to be L= 50.9 {+-}3.1 cm for the following graphite characteristics: density = 1.7 g/cm{sup 3}; boron content = 0.1 ppm; absorption cross section = 3.7 mb.

  8. A standard graphite block

    International Nuclear Information System (INIS)

    Ivkovic, M.; Zdravkovic, Z.; Sotic, O.

    1966-04-01

    A graphite block was calibrated for the thermal neutron flux of the Ra-Be source using indium foils as detectors. Experimental values of the thermal neutron flux along the central vertical axis of the system were corrected for the self-shielding effect and depression of flux in the detector. The experimental values obtained were compared with the values calculated on the basis of solving the conservation neutron equation by the continuous slowing-down theory. In this theoretical calculation of the flux the Ra-Be source was divided into three resonance energy regions. The measurement of the thermal neutron diffusion length in the standard graphite block is described. The measurements were performed in the thermal neutron region of the system. The experimental results were interpreted by the diffusion theory for point thermal neutron source in the finite system. The thermal neutron diffusion length was calculated to be L= 50.9 ±3.1 cm for the following graphite characteristics: density = 1.7 g/cm 3 ; boron content = 0.1 ppm; absorption cross section = 3.7 mb

  9. 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.

  10. [The electric furnace of Henri Moissan at one hundred years: connection with the electric furnace, the solar furnace, the plasma furnace?].

    Science.gov (United States)

    Royère, C

    1999-03-01

    The trace of Henri Moissan's pioneer work 100 years ago is clearly evidenced by an overview of achievements in high temperature devices; 1987: "Le four électrique" by Henri Moissan; 1948-1952: "High temperature heating in a cavity rotary kiln using focusing of solar radiation" by Félix Trombe; 1962: "The cavity rotary kiln using focused solar radiation jointly with a plasma gun" by Marc Foëx; 1970: "The rotary kiln with two plasma guns and arc transfer" by Marc Foëx; 1984: "The plasma furnace" by Electricité de France (EDF) at Renardières; 1997: "The plasma furnace" by the Atomic Energy Center (CEA) at Cadarache, the VULCANO program. The first part of this contribution is devoted to Henri Moissan. Re-reading his early book on the electric furnace, especially the first chapter and the sections on silica, carbon vapor and experiments performed in casting molten metal--the conclusions are outstanding--provides modern readers with an amazing insight into future developments. The last two parts are devoted to Félix Trombe and Marc Foëx, tracing the evolution of high temperature cavity processus leading to the solar furnace and the present day plasma furnace at the CEA. Focus is placed on research conducted by the French National Center for Scientific Research (CNRS) with the solar and plasma furnaces at Odeillo. The relationships with Henri Moissan's early work are amazing, offering a well deserved homage to this pioneer researcher.

  11. Energy Saving in Industrial Annealing Furnaces

    Directory of Open Access Journals (Sweden)

    Fatma ÇANKA KILIÇ

    2018-03-01

    Full Text Available In this study, an energy efficiency studies have been carried out in a natural gas-fired rolling mill annealing furnace of an industrial establishment. In this context, exhaust gas from the furnace has been examined in terms of waste heat potential. In the examinations that have been made in detail; waste heat potential was found as 3.630,31 kW. Technical and feasibility studies have been carried out to realize electricity production through an Organic Rankine Cycle (ORC system for evaluating the waste heat potential of the annealing furnace. It has been calculated that 1.626.378,88 kWh/year of electricity can be generated by using the exhaust gas waste heat of the annealing furnace through an ORC system to produce electric energy with a net efficiency of 16%. The financial value of this energy was determined as 436.032,18 TL/year and the simple repayment period of the investment was 8,12 years. Since the annealing period of the annealing furnace is 2800 hours/year, the investment has not been found to be feasible in terms of the feasibility studies. However, the investment suitability can be assured when the annealing furnace is operating at full capacity for 8,000 hours or more annually.

  12. Structural disorder of graphite and implications for graphite thermometry

    Science.gov (United States)

    Kirilova, Martina; Toy, Virginia; Rooney, Jeremy S.; Giorgetti, Carolina; Gordon, Keith C.; Collettini, Cristiano; Takeshita, Toru

    2018-02-01

    Graphitization, or the progressive maturation of carbonaceous material, is considered an irreversible process. Thus, the degree of graphite crystallinity, or its structural order, has been calibrated as an indicator of the peak metamorphic temperatures experienced by the host rocks. However, discrepancies between temperatures indicated by graphite crystallinity versus other thermometers have been documented in deformed rocks. To examine the possibility of mechanical modifications of graphite structure and the potential impacts on graphite thermometry, we performed laboratory deformation experiments. We sheared highly crystalline graphite powder at normal stresses of 5 and 25 megapascal (MPa) and aseismic velocities of 1, 10 and 100 µm s-1. The degree of structural order both in the starting and resulting materials was analyzed by Raman microspectroscopy. Our results demonstrate structural disorder of graphite, manifested as changes in the Raman spectra. Microstructural observations show that brittle processes caused the documented mechanical modifications of the aggregate graphite crystallinity. We conclude that the calibrated graphite thermometer is ambiguous in active tectonic settings.

  13. Structural disorder of graphite and implications for graphite thermometry

    Directory of Open Access Journals (Sweden)

    M. Kirilova

    2018-02-01

    Full Text Available Graphitization, or the progressive maturation of carbonaceous material, is considered an irreversible process. Thus, the degree of graphite crystallinity, or its structural order, has been calibrated as an indicator of the peak metamorphic temperatures experienced by the host rocks. However, discrepancies between temperatures indicated by graphite crystallinity versus other thermometers have been documented in deformed rocks. To examine the possibility of mechanical modifications of graphite structure and the potential impacts on graphite thermometry, we performed laboratory deformation experiments. We sheared highly crystalline graphite powder at normal stresses of 5 and 25  megapascal (MPa and aseismic velocities of 1, 10 and 100 µm s−1. The degree of structural order both in the starting and resulting materials was analyzed by Raman microspectroscopy. Our results demonstrate structural disorder of graphite, manifested as changes in the Raman spectra. Microstructural observations show that brittle processes caused the documented mechanical modifications of the aggregate graphite crystallinity. We conclude that the calibrated graphite thermometer is ambiguous in active tectonic settings.

  14. Comparison of a burning mass ceramics coating in laboratory furnace and instrustrial furnace; Comparacao de queimas de uma massa ceramica de revestimento em forno de laboratorio e forno industrial

    Energy Technology Data Exchange (ETDEWEB)

    Soares, R.A.L., E-mail: robertoarruda@ifpi.edu.br [Instituto Federal de Educacao, Ciencia e Tecnologia do Piaui (IFPI), Terersina, PI (Brazil); Castro, J.R. de S. [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil)

    2012-07-01

    This work intends to analyze the differences obtained in the technological properties of a ceramic coating after firing in two distinct environments, laboratory furnace and industrial furnace. For this, was characterized a ceramic mass used in the production of porous coating. The analyzes were performed chemical, mineralogical and thermal mass in that. The specimens were obtained by compacting and burned in the maximum temperature of 1140 deg C in two furnaces, laboratory and industrial. The technological tests were performed linear shrinkage, water absorption, bulk density and mechanical strength. The microstructure was evaluated by ray-X diffraction and scanning electron microscopy. The results showed that both furnaces provided significant differences in analyzed specimens, such as increased strength and low water absorption in the fired samples in a laboratory furnace, for example. (author)

  15. 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.

  16. Chemical stabilization of graphite surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Bistrika, Alexander A.; Lerner, Michael M.

    2018-04-03

    Embodiments of a device, or a component of a device, including a stabilized graphite surface, methods of stabilizing graphite surfaces, and uses for the devices or components are disclosed. The device or component includes a surface comprising graphite, and a plurality of haloaryl ions and/or haloalkyl ions bound to at least a portion of the graphite. The ions may be perhaloaryl ions and/or perhaloalkyl ions. In certain embodiments, the ions are perfluorobenzenesulfonate anions. Embodiments of the device or component including stabilized graphite surfaces may maintain a steady-state oxidation or reduction surface current density after being exposed to continuous oxidation conditions for a period of at least 1-100 hours. The device or component is prepared by exposing a graphite-containing surface to an acidic aqueous solution of the ions under oxidizing conditions. The device or component can be exposed in situ to the solution.

  17. Selective extraction of chromium(VI) using a leaching procedure with sodium carbonate from some plant leaves, soil and sediment samples

    Energy Technology Data Exchange (ETDEWEB)

    Elci, Latif, E-mail: elci@pamukkale.edu.tr [Department of Chemistry, Pamukkale University, 20017 Denizli (Turkey); Divrikli, Umit; Akdogan, Abdullah; Hol, Aysen; Cetin, Ayse [Department of Chemistry, Pamukkale University, 20017 Denizli (Turkey); Soylak, Mustafa [Department of Chemistry, Erciyes University, 38039 Kayseri (Turkey)

    2010-01-15

    Speciation of chromium in some plant leaves, soil and sediment samples was carried out by selective leaching of Cr(VI) using a sodium carbonate leaching procedure. Total chromium from the samples was extracted using aqua regia and oxidative acid digestion, respectively. The concentrations of chromium species in the extracts were determined using by graphite furnace atomic absorption spectrometry (GFAAS). Uncoated graphite furnace tubes were used as an atomizer. Due to the presence of relatively high amounts of Na{sub 2}CO{sub 3} in the resulting samples, the possible influences of Na{sub 2}CO{sub 3} on the absorbance signals were checked. There is no interference of Na{sub 2}CO{sub 3} on the chromium absorbance up to 0.1 mol L{sup -1} Na{sub 2}CO{sub 3}. A limit of detection (LOD) for determination of Cr(VI) in 0.1 Na{sub 2}CO{sub 3} solution by GFAAS was found to be 0.93 {mu}g L{sup -1}. The procedure was applied to environmental samples. The relative standard deviation, R.S.D. as precision for 10 replicate measurements of 20 {mu} L{sup -1} Cr in processed soil sample was 4.2%.

  18. Selective extraction of chromium(VI) using a leaching procedure with sodium carbonate from some plant leaves, soil and sediment samples.

    Science.gov (United States)

    Elci, Latif; Divrikli, Umit; Akdogan, Abdullah; Hol, Aysen; Cetin, Ayse; Soylak, Mustafa

    2010-01-15

    Speciation of chromium in some plant leaves, soil and sediment samples was carried out by selective leaching of Cr(VI) using a sodium carbonate leaching procedure. Total chromium from the samples was extracted using aqua regia and oxidative acid digestion, respectively. The concentrations of chromium species in the extracts were determined using by graphite furnace atomic absorption spectrometry (GFAAS). Uncoated graphite furnace tubes were used as an atomizer. Due to the presence of relatively high amounts of Na(2)CO(3) in the resulting samples, the possible influences of Na(2)CO(3) on the absorbance signals were checked. There is no interference of Na(2)CO(3) on the chromium absorbance up to 0.1 mol L(-1) Na(2)CO(3). A limit of detection (LOD) for determination of Cr(VI) in 0.1 Na(2)CO(3) solution by GFAAS was found to be 0.93 microg L(-1). The procedure was applied to environmental samples. The relative standard deviation, R.S.D. as precision for 10 replicate measurements of 20 microL(-1) Cr in processed soil sample was 4.2%.

  19. Comparison of the oxidation rate and degree of graphitization of selected IG and NBG nuclear graphite grades

    Science.gov (United States)

    Chi, Se-Hwan; Kim, Gen-Chan

    2008-10-01

    The oxidation rate and degree of graphitization (DOG) were determined for some selected nuclear graphite grades (i.e., IG-110, IG-430, NBG-18, NBG-25) and compared in view of their filler coke type (i.e., pitch or petroleum coke) and the physical property of the grades. Oxidation rates were determined at six temperatures between 600 and 960 °C in air by using a three-zone vertical tube furnace at a 10 l/min air flow rate. The specimens were a cylinder with a 25.4 mm diameter and a 25.4 mm length. The DOG was determined based on the lattice parameter c determined from an X-ray diffraction (XRD). Results showed that, even though the four examined nuclear graphite grades showed a highly temperature-sensitive oxidation behavior through out the test temperature range of 600-950 °C, the differences between the grades were not significant. The oxidation rates determined for a 5-10% weight loss at the six temperatures were nearly the same except for 702 and 808 °C, where the pitch coke graphites showed an apparent decrease in their oxidation rate, more so than the petroleum coke graphites. These effects of the coke type reduced or nearly disappeared with an increasing temperature. The average activation energy determined for 608-808 °C was 161.5 ± 7.3 kJ/mol, showing that the dominant oxidation reaction occurred by a chemical control. A relationship between the oxidation rate and DOG was not observed.

  20. Comparison of the oxidation rate and degree of graphitization of selected IG and NBG nuclear graphite grades

    International Nuclear Information System (INIS)

    Chi, Se-Hwan; Kim, Gen-Chan

    2008-01-01

    The oxidation rate and degree of graphitization (DOG) were determined for some selected nuclear graphite grades (i.e., IG-110, IG-430, NBG-18, NBG-25) and compared in view of their filler coke type (i.e., pitch or petroleum coke) and the physical property of the grades. Oxidation rates were determined at six temperatures between 600 and 960 deg. C in air by using a three-zone vertical tube furnace at a 10 l/min air flow rate. The specimens were a cylinder with a 25.4 mm diameter and a 25.4 mm length. The DOG was determined based on the lattice parameter c determined from an X-ray diffraction (XRD). Results showed that, even though the four examined nuclear graphite grades showed a highly temperature-sensitive oxidation behavior through out the test temperature range of 600-950 deg. C, the differences between the grades were not significant. The oxidation rates determined for a 5-10% weight loss at the six temperatures were nearly the same except for 702 and 808 deg. C, where the pitch coke graphites showed an apparent decrease in their oxidation rate, more so than the petroleum coke graphites. These effects of the coke type reduced or nearly disappeared with an increasing temperature. The average activation energy determined for 608-808 deg. C was 161.5 ± 7.3 kJ/mol, showing that the dominant oxidation reaction occurred by a chemical control. A relationship between the oxidation rate and DOG was not observed

  1. 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.

  2. 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....

  3. Preparation and Characterization of Graphite Waste/CeO2 Composites

    Science.gov (United States)

    Kusrini, E.; Utami, C. S.; Nasruddin; Prasetyanto, E. A.; Bawono, Aji A.

    2018-03-01

    In this research, the chemical modification of graphite waste with CeO2 was developed and characterized. Graphite waste was pretreated with mechanical to obtain the size 200 mesh (75 μm), and thermal methods at 110°C oven for 6 hours. Here, we demonstrate final properties of graphite before modification (GBM), activated graphite (GA) and graphite/CeO2 composite with variation of 0.5, 1 and 2 g of CeO2 (G0.5; G1; G2). The effect of CeO2 concentration was observed. The presence of cerium in modified graphite samples (G0.5; G1; G2) were analyzed using SEM-EDX. The results show that the best surface area was found in G2 is 26.82 m2/g. The presence of CeO2 onto graphite surface does not significantly increase the surface area of composites.

  4. Study on "1"4C content in post-irradiation graphite spheres of HTR-10

    International Nuclear Information System (INIS)

    Wang Shouang; Pi Yue; Xie Feng; Li Hong; Cao Jianzhu

    2014-01-01

    Since the production mechanism of the "1"4C in spherical fuel elements was similar to that of fuel-free graphite spheres, in order to obtain the amount of "1"4C in fuel elements and graphite spheres of HTR-10, the production mechanism of the "1"4C in graphite spheres was studied. The production sources of the "1"4C in graphite spheres and fuel elements were summarized, the amount of "1"4C in the post-irradiation graphite spheres was calculated, the decomposition techniques of graphite spheres were compared, and experimental methods for decomposing the graphite spheres and preparing the "1"4C sample were proposed. The results can lay the foundation for further experimental research and provide theoretical calculations for comparison. (authors)

  5. The determination of oxygen in metals using an impulse heating furnace with a simple transfer lock

    International Nuclear Information System (INIS)

    Dale, L.S.; de Jong, S.; Kelly, J.W.; Whittem, R.N.

    1975-05-01

    An impulse heating furnace has been constructed for the determination of low levels of oxygen down to 100 μg g -1 in metals. The furnace is equipped with a sample transfer lock which permits samples to be loaded into outgassed crucibles in a helium atmosphere. As a result, blank levels in the range 2 to 3 μg oxygen are obtained; the modification also results in shorter sample processing time. The apparatus is described, and its suitability for oxygen determinations at these levels has been verified by comparison of results obtained on reference and analysed materials. (author)

  6. Industrial furnace with improved heat transfer

    Energy Technology Data Exchange (ETDEWEB)

    Hoetzl, M.; Lingle, T.M.

    1993-07-20

    A method is described for effecting improved heat transfer with in an industrial furnace having a cylindrical furnace section, a door at one end of the furnace section, an end plate at the opposite end of the section a circular fan plate concentrically positioned within the furnace section to define a cylindrical fan chamber between the plate and the end section with a fan there between and a heat treat chamber between the plate and the door, the fan plate defining a non-orificing annular space extending between the interior of the cylindrical furnace section and the outer edge of the plate, the plate having a centrally located under-pressure opening extending there through and a plurality of circumferentially spaced tubular heating elements extending through the annular space into the heat treating chamber, the method comprising the steps of: (a) heating the heating elements to a temperature which is hotter that the temperature of the work within the heat treating chamber; (b) rotating the fan at a speed sufficient to form a portion of the furnace atmosphere as a wind mass swirling about the fan chamber; (c) propagating the wind mass through the annular space into the heat treating chamber as a swirling wind mass in the form of an annulus, the wind mass impinging the heating elements to establish heat transfer contact therewith while the mass retains its annulus shape until contacting the door and without any significant movement of the wind mass into the center of the heat treating chamber; (d) drawing the wind mass through the under-pressure zone after the wind mass comes into heat transfer contact with the work in the heat treating chamber; and (e) thereafter heating the work by radiation from the beating elements at high furnace temperatures in excess of about 1,600 F.

  7. Spectroscopical determination of impurities in nuclear graphite

    International Nuclear Information System (INIS)

    Lordello, A.R.; Tognini, R.P.

    1975-01-01

    A spectrochemical method for the direct determination of B, Cd, Si, Hg, Fe, Mg, Mn, Cr, Ni, Al, Mo, Ti, Sr, Na, Zn, and As in nuclear grade graphite is described. A 9:1 ratio of graphite to copper difluoride is used in the preparation of samples and standards. The excitation is carried out in a d-c at 10 amperes. The copper fluoride used as spectrographic buffer serves to increase the volatilization rate of the impurities and to diminish the differences in the nature of the analytical and calibration samples. The relative standard deviations for the determination of the 16 trace elements, except Sr, Fe, Cd, Al and Si, are in the range of 8 - 20% in their appropriate calibration levels. For the latter five elements they are approximately 20-40%

  8. Assessment of management modes for graphite from reactor decommissioning

    International Nuclear Information System (INIS)

    White, I.F.; Smith, G.M.; Saunders, L.J.; Kaye, C.J.; Martin, T.J.; Clarke, G.H.; Wakerley, M.W.

    1984-01-01

    A technological and radiological assessment has been made of the management options for irradiated graphite wastes from the decommissioning of Magnox and advanced gas-cooled reactors. Detailed radionuclide inventories have been estimated, the main contribution being from activation of the graphite and its stable impurities. Three different packaging methods for graphite have been described; each could be used for either sea or land disposal, is logistically feasible and could be achieved at reasonable cost. Leaching tests have been carried out on small samples of irradiated graphite under a variety of conditions including those of the deep ocean bed; the different conditions had little effect on the observed leach rates of radiologically significant radionuclides. Radiological assessments were made of four generic options for disposal of packaged graphite: on the deep ocean bed, in deep geologic repositories at two different types of site, and by shallow land burial. Incineration of graphite was also considered, though this option presents logistical problems. With appropriate precautions during the lifetime of the Cobalt-60 content of the graphite, any of the options considered could give acceptably low doses to individuals, and all would merit further investigation in site-specific contexts

  9. Immobilization of individual nanotubes in graphitic layers for electrical characterization

    International Nuclear Information System (INIS)

    Roy, Debmalya; Tiwari, Neeru; Mukhopadhyay, K; Saxena, A K

    2014-01-01

    A simple route is followed to produce an abundance of individual carbon nanotubes (CNTs) immobilized in graphitic layers to counter the challenge of locating individual CNTs and restrict the lateral displacement of CNTs due to the high electrostatic force exerted by a scanning tunnelling microscope tip for electrical characterization. Graphitic layers are selected for the embedding matrix as graphite and the nanotubes have a similar work function and hence would not perturb the electrical configuration of the nanotube. Solvent mediated exfoliation of graphite layers to insert the nanotubes was preferred over oxidative expansion, as oxidation could perturb the electrical configuration of graphite. During the exfoliation of graphite the optimized amount of nanotubes was introduced into the medium such that an individual nanotube could be immobilized in few-layer graphene followed by precipitation and centrifugation. The dose and the time of sonication were optimized to ensure that damage to the walls of the nanotubes is minimized, although the ultrasonication causes scissoring of the nanotube length. This procedure for immobilizing nanotubes in graphitic layers would be equally applicable for functionalized CNTs as well. The capability of embedding individual nanotubes into a similar work function material in an organic solvent, which could then be transferred onto a substrate by simple drop casting or spin coating methods, has an added advantage in sample preparation for the STM characterization of CNTs. (paper)

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

    Science.gov (United States)

    Zeng, Fan W.; Han, Karen; Olasov, Lauren R.; Gallego, Nidia C.; Contescu, Cristian I.; Spicer, James B.

    2015-05-01

    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.

  11. Effect of various dopant elements on primary graphite growth

    International Nuclear Information System (INIS)

    Valle, N; Theuwissen, K; Lacaze, J; Sertucha, J

    2012-01-01

    Five spheroidal graphite cast irons were investigated, a usual ferritic grade and four pearlitic alloys containing Cu and doped with Sb, Sn and Ti. These alloys were remelted in a graphite crucible, leading to volatilization of the magnesium added for spheroidization and to carbon saturation of the liquid. The alloys were then cooled down and maintained at a temperature above the eutectic temperature. During this step, primary graphite could develop showing various features depending on the doping elements added. The largest effects were that of Ti which greatly reduces graphite nucleation and growth, and that of Sb which leads to rounded agglomerates instead of lamellar graphite. The samples have been investigated with secondary ion mass spectrometry to enlighten distribution of elements in primary graphite. SIMS analysis showed almost even distribution of elements, including Mg and Al (from the inoculant) in the ferritic grade, while uneven distribution was evident in all doped alloys. Investigations are going on to clarify if the uneven distribution is associated with structural defects in the graphite precipitates.

  12. RBS investigations of high-temperature reactions on graphite substrates

    Energy Technology Data Exchange (ETDEWEB)

    Eloi, C.C. [Kentucky Univ., Lexington, KY (United States). Dept. of Chemistry]|[Center for Applied Energy Research, University of Kentucky, Lexington, KY 40506 (United States); Robertson, J.D. [Kentucky Univ., Lexington, KY (United States). Dept. of Chemistry]|[Center for Applied Energy Research, University of Kentucky, Lexington, KY 40506 (United States); Majidi, V. [Kentucky Univ., Lexington, KY (United States). Dept. of Chemistry

    1995-05-01

    While graphite furnace atomic absorption spectrometry (GFAAS) is one of the most powerful techniques for ultratrace analysis of Pb, it is often plagued by matrix interferences. These interferences are minimized by the addition of matrix modifiers which stabilize the analyte signal through unknown mechanisms. Using RBS, the high temperature reactions of nitrate salts of Pb were studied on pyrolytically coated graphite with and without matrix modifiers. The addition of an ammonium phosphate modifier was found to stabilize Pb through the formation of a metal oxy-phosphorus compound. Moreover, the depth profiles demonstrated that the pyrolytically coated graphite was not impervious as previously thought. Pre-treatment of the surface with O{sub 2} is also known to cause a delay in the vaporization of Pb. While a surface effect had previously been postulated, the 3.04 MeV resonance {sup 16}O({alpha}, {alpha}){sup 16}O elastic scattering measurements show that it proceeds through the formation of surface bound lead-oxygen species as the number of oxygen atoms chemisorbed and the number of lead atoms, present on the surface prior to vaporization, are nearly equal. (orig.).

  13. Product Evaluation Task Force Phase Two report for CAGR graphite

    International Nuclear Information System (INIS)

    Francis, A.J.; Davies, A.

    1991-01-01

    It has been proposed that all Intermediate Level Wastes arising at Sellafield should be encapsulated prior to ultimate disposal. The Product Evaluation Task Force (PETF) was set up to investigate possible encapsulants and to produce an adequate data base to justify the preferred matrices. This report details the work carried out under Phase 2 of the Product Evaluation Task Force programme, on CAGR graphite. Three possible types of encapsulants for CAGR graphites:-Inorganic cements, Polymer cements and Polymers are evaluated using the Kepner Tregoe decision analysis technique. This technique provides a methodology for scoring and ranking alternative options and evaluating any risks associated with an option. The analysis shows that for all four stages of waste management operations ie Storage, Transport, handling and emplacement, Disposal and Process, cement matrices are considerably superior to other potential matrices. A matrix, consisting of three parts Blast Furnace Slag (BFS) to one part Ordinary Portland Cement (OPC) is recommended as the preferred matrix for Phase 3 studies on CAGR graphite. (author)

  14. Management of UKAEA graphite liabilities

    International Nuclear Information System (INIS)

    Wise, M.

    2001-01-01

    The UK Atomic Energy Authority (UKAEA) is responsible for managing its liabilities for redundant research reactors and other active facilities concerned with the development of the UK nuclear technology programme since 1947. These liabilities include irradiated graphite from a variety of different sources including low irradiation temperature reactor graphite (the Windscale Piles 1 and 2, British Energy Pile O and Graphite Low Energy Experimental Pile at Harwell and the Material Testing Reactors at Harwell and Dounreay), advanced gas-cooled reactor graphite (from the Windscale Advanced Gas-cooled Reactor) and graphite from fast reactor systems (neutron shield graphite from the Dounreay Prototype Fast Reactor and Dounreay Fast Reactor). The decommissioning and dismantling of these facilities will give rise to over 6,000 tonnes of graphite requiring disposal. The first graphite will be retrieved from the dismantling of Windscale Pile 1 and the Windscale Advanced Gas-cooled Reactor during the next five years. UKAEA has undertaken extensive studies to consider the best practicable options for disposing of these graphite liabilities in a manner that is safe whilst minimising the associated costs and technical risks. These options include (but are not limited to), disposal as Low Level Waste, incineration, or encapsulation and disposal as Intermediate Level Waste. There are a number of technical issues associated with each of these proposed disposal options; these include Wigner energy, radionuclide inventory determination, encapsulation of graphite dust, galvanic coupling interactions enhancing the corrosion of mild steel and public acceptability. UKAEA is currently developing packaging concepts and designing packaging plants for processing these graphite wastes in consultation with other holders of graphite wastes throughout Europe. 'Letters of Comfort' have been sought from both the Low Level Waste and the Intermediate Level Waste disposal organisations to support the

  15. Analysis of graphite gasification by water vapor at different conversions

    International Nuclear Information System (INIS)

    Xiaowei, Luo; Xiaoyu, Yu; Suyuan, Yu; Jean-Charles, Robin

    2014-01-01

    Highlights: • Graphite was gasified at different conversions. • The reaction temperature influences on the dimensionless the reaction rate. • The thickness or radius influence on the dimensionless reaction rate. - Abstract: The gasification rate of porous solids varies with the conversions with the rate increasing to a maximum and then decreasing. Many graphite gasification experiments have illustrated that the maximum gasification rates occur at different conversions for different temperatures and sample geometries. Thus, the gasification rate is related to the conversion, temperature and geometry of the graphite. The influences of those factors were studied for the graphite gasification by water vapor. A theoretical analysis was done on the basis of several logical assumptions. The influence of temperatures on the reaction rate was investigated for plate-like and cylindrical graphite. The effects of thickness for a plate-like graphite sample and of radius for a cylindrical sample on the reaction rate were also studied theoretically. The results reveal that the maximum dimensionless reaction rate decreases with reaction temperature. The plate thickness or the cylinder radius also affects the maximum dimensionless reaction rate

  16. 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...

  17. 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

  18. Modification of structural graphite machining

    International Nuclear Information System (INIS)

    Lavrenev, M.M.

    1979-01-01

    Studied are machining procedures for structural graphites (GMZ, MG, MG-1, PPG) most widely used in industry, of the article mass being about 50 kg. Presented are dependences necessary for the calculation of cross sections of chip suction tappers and duster pipelines in machine shops for structural graphite machining

  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. Glass-Graphite Composite Materials

    International Nuclear Information System (INIS)

    Mayzan, M.Z.H.; Lloyd, J.W.; Heath, P.G.; Stennett, M.C.; Hyatt, N.C.; Hand, R.J.

    2016-01-01

    A summary is presented of investigations into the potential of producing glass-composite materials for the immobilisation of graphite or other carbonaceous materials arising from nuclear power generation. The methods are primarily based on the production of base glasses which are subsequently sintered with powdered graphite or simulant TRISO particles. Consideration is also given to the direct preparation of glass-graphite composite materials using microwave technology. Production of dense composite wasteforms with TRISO particles was more successful than with powdered graphite, as wasteforms containing larger amounts of graphite were resistant to densification and the glasses tried did not penetrate the pores under the pressureless conditions used. Based on the results obtained it is concluded that the production of dense glassgraphite composite wasteforms will require the application of pressure. (author)

  1. Continuous austempering fluidized bed furnace. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Srinivasan, M.N. [Lamar Univ., Beaumont, TX (United States). Dept. of Mechanical Engineering

    1997-09-23

    The intended objective of this project was to show the benefits of using a fluidized bed furnace for austenitizing and austempering of steel castings in a continuous manner. The division of responsibilities was as follows: (1) design of the fluidized bed furnace--Kemp Development Corporation; (2) fabrication of the fluidized bed furnace--Quality Electric Steel, Inc.; (3) procedure for austempering of steel castings, analysis of the results after austempering--Texas A and M University (Texas Engineering Experiment Station). The Department of Energy provided funding to Texas A and M University and Kemp Development Corporation. The responsibility of Quality Electric Steel was to fabricate the fluidized bed, make test castings and perform austempering of the steel castings in the fluidized bed, at their own expense. The project goals had to be reviewed several times due to financial constraints and technical difficulties encountered during the course of the project. The modifications made and the associated events are listed in chronological order.

  2. 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

  3. Thermal strain measurements in graphite using electronic speckle pattern interferometry

    International Nuclear Information System (INIS)

    Tamulevicius, S.; Augulis, L.; Augulis, R.; Zabarskas, V.; Levinskas, R.; Poskas, P.

    2001-01-01

    Two 1500 MW(e) RBMK Units are operated at Ignalina NPP in Lithuania. Due to recent decision of the Parliament on the earlier closure of Unit 1, preparatory work for decommissioning have been initiated. Preferred decommissioning strategy is based on delayed dismantling after rather long safe enclosure period. Since graphite is one of the basic and probably the most voluminous components of the reactor internals, a sufficient information on status and behaviour of graphite moderator and reflector during long time safe enclosure period is of special significance. In this context, thermal strain in graphite is one of the parameters requiring particular interest. Electronic speckle pattern interferometry has been proposed and successfully tested to control this parameter using the real samples of graphite from Ignalina NPP Units. (author)

  4. Porosity effects in the neutron total cross section of graphite

    International Nuclear Information System (INIS)

    Santisteban, J. R; Dawidowski, J; Petriw, S. N

    2009-01-01

    Graphite has been used in nuclear reactors since the birth of the nuclear industry due to its good performance as a neutron moderator material. Graphite is still an option as moderator for generation IV reactors due to its good mechanical and thermal properties at high operation temperatures. So, there has been renewed interest in a revision of the computer libraries used to describe the neutron cross section of graphite. For sub-thermal neutron energies, polycrystalline graphite shows a larger total cross section (between 4 and 8 barns) than predicted by existing theoretical models (0.2 barns). In order to investigate the origin of this discrepancy we measured the total cross section of graphite samples of three different origins, in the energy range from 0.001 eV to 10 eV. Different experimental arrangements and sample treatments were explored, to identify the effect of various experimental parameters on the total cross section measurement. The experiments showed that the increase in total cross section is due to neutrons scattered around the forward direction. We associate these small-angle scattered neutrons (SANS) to the porous structure of graphite, and formulate a very simple model to compute its contribution to the total cross section of the material. This results in an analytic expression that explicitly depends on the density and mean size of the pores, which can be easily incorporated in nuclear library codes. [es

  5. 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.

  6. Design of a rotating-hearth furnace

    Energy Technology Data Exchange (ETDEWEB)

    Behrens, H A [LOI Industrieofenanlagen G.m.b.H., Essen (Germany, F.R.)

    1979-09-01

    Part I of this paper is intended to present a review of the theory of heating round stock of a length considerably exceeding the diameter. It is permissible to neglect heating from the ends of the cylinders. With short and thick ingots as used in pilgrim mills, for instance, such simplification is not possible. The method for calculating the waste gas temperature can also be used for the remaining furnace sections provided certain conditions are allowed for and computational procedures observed. Part II of the paper will deal with this and with the major design features of rotating-hearth furnaces.

  7. Process and furnace for working bituminous materials

    Energy Technology Data Exchange (ETDEWEB)

    Klotzer, M

    1921-06-28

    A process for working up bitumen-containing materials, such as coal, peat and shale is characterized in that the material in thin-height batches with constant shaking by means of forward and backward movement of an elongated horizontal hearth heated underneath on which the material freely lies and on which it is moved in the furnace, through a single narrow furnace space with zone-wise heating of the hearth. A drying zone, a spent-material removal zone, and a carbonization zone are provided. Under separate hoods the gases and vapors are removed from these zones.

  8. 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.

  9. Glass Furnace Project, October 1982-March 1983

    International Nuclear Information System (INIS)

    Armstrong, K.M.; Klingler, L.M.

    1983-01-01

    In the Glass Furnace Project currently under way at Mound, a treatment technology for low-level radioactive waste is being evaluated that will combine volume reduction and immobilization in one step. Initial work focused on demonstrating the ability of the furnace to efficiently incinerate nonradioactive, simulated power-plant waste and on determining the adequacy of immobilization in a soda-lime silica matrix. Further evaluation of the system will involve a demonstration of the combustion and containment of radioactive waste. In preparation for this next phase of the program, preliminary investigation and design work were conducted during the past six months. 5 figures, 1 table

  10. 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.

  11. Dry Sliding Wear Behavior of Spark Plasma Sintered Fe-Based Bulk Metallic Glass/Graphite Composites

    Directory of Open Access Journals (Sweden)

    Xiulin Ji

    2016-09-01

    Full Text Available Bulk metallic glass (BMG and BMG-graphite composites were fabricated using spark plasma sintering at the sintering temperature of 575 °C and holding time of 15 min. The sintered composites exhibited partial crystallization and the presence of distributed porosity and graphite particles. The effect of graphite reinforcement on the tribological properties of the BMG/graphite composites was investigated using dry ball-on-disc sliding wear tests. The reinforcement of graphite resulted in a reduction in both the wear rate and the coefficient of friction as compared to monolithic BMG samples. The wear surfaces of BMG/graphite composites showed regions of localized wear loss due to microcracking and fracture, as was also the case with the regions covered with graphite-rich protective film due to smearing of pulled off graphite particles.

  12. Imaging of tritium implanted into graphite

    International Nuclear Information System (INIS)

    Malinowski, M.E.; Causey, R.A.

    1988-01-01

    The extensive use of graphite in plasma-facing surfaces of tokamaks such as the Tokamak Fusion Test Reactor, which has planned tritium discharges, makes two-dimensional tritium detection techniques important in helping to determine torus tritium inventories. We have performed experiments in which highly oriented pyrolytic graphite (HOPG) samples were first tritium implanted with fluences of ∼10 16 T/cm 2 at energies approx. 0 C resulted in no discernible motion of tritium along the basal plane, but did show that significant desorption of the implanted tritium occurred. The current results indicate that tritium in quantities of 10 12 T/cm 2 in tritiated components could be readily detected by imaging at lower magnifications

  13. 3D Numerical Analysis of the Arc Plasma Behavior in a Submerged DC Electric Arc Furnace for the Production of Fused MgO

    International Nuclear Information System (INIS)

    Wang Zhen; Wang Ninghui; Li Tie; Cao Yong

    2012-01-01

    A three dimensional steady-state magnetohydrodynamic model is developed for the arc plasma in a DC submerged electric arc furnace for the production of fused MgO. The arc is generated in a small semi-enclosed space formed by the graphite electrode, the molten bath and unmelted raw materials. The model is first used to solve a similar problem in a steel making furnace, and the calculated results are found to be in good agreement with the published measurements. The behavior of arcs with different arc lengths is also studied in the furnace for MgO production. From the distribution of the arc pressure on the bath surface it is shown that the arc plasma impingement is large enough to cause a crater-like depression on the surface of the MgO bath. The circulation of the high temperature air under the electrode may enhance the arc efficiency, especially for a shorter arc.

  14. Radionuclide characterization of graphite stacks from plutonium production reactors of the Siberian group of chemical enterprises

    International Nuclear Information System (INIS)

    Bushuev, A.V.; Verzilov, Yu.M.; Zubarev, V.N.

    2001-01-01

    The residual radionuclide concentrations and distributions in graphite from moderator stack of plutonium production reactors at Tomsk-7 have been investigated. It was found that the dominant activity of graphite is 14 C. To gain information on surface and volume contamination of graphite blocks from the moderator stack, the special sets of samples were collected and assayed. The schemes are proposed for evaluation of individual radionuclide inventories together with results of the evaluations performed. (author)

  15. 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.

  16. Hypervelocity impacts into graphite

    International Nuclear Information System (INIS)

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

    2011-01-01

    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.

  17. Acoustic emission from polycrystalline graphites

    International Nuclear Information System (INIS)

    Ioka, I.; Yoda, S.; Oku, T.; Miyamoto, Y.

    1987-01-01

    Acoustic emission was monitored from polycrystalline graphites with different microstructure (pore size and pore volume) subjected to compressive loading. The graphites used in this study comprised five brands, that is, PGX, ISEM-1, IG-11, IG-15, and ISO-88. A root mean square (RMS) voltage and event counts of acoustic emission for graphites were measured during compressive loading. The acoustic emission was measured using a computed-based data acquisition and analysis system. The graphites were first deformed up to 80 % of the average fracture stress, then unloaded and reloaded again until the fracture occured. During the first loading, the change in RMS voltage for acoustic emission was detected from the initial stage. During the unloading, the RMS voltage became zero level as soon as the applied stress was released and then gradually rose to a peak and declined. The behavior indicated that the reversed plastic deformation occured in graphites. During the second loading, the RMS voltage gently increased until the applied stress exceeded the maximum stress of the first loading; there is no Kaiser effect in the graphites. A bicrystal model could give a reasonable explanation of this results. The empirical equation between the ratio of σ AE to σ f and σ f was obtained. It is considered that the detection of microfracture by the acoustic emission technique is effective in macrofracture prediction of polycrystalline graphites. (author)

  18. BPM Motors in Residential Gas Furnaces: What are the Savings?

    OpenAIRE

    Lutz, James; Franco, Victor; Lekov, Alex; Wong-Parodi, Gabrielle

    2006-01-01

    Residential gas furnaces contain blowers to distribute warm air. Currently, furnace blowers use either a Permanent Split Capacitor (PSC) or a Brushless Permanent Magnet (BPM) motor. Blowers account for the majority of furnace electricity consumption. Therefore, accurate determination of the blower electricity consumption is important for understanding electricity consumption of furnaces. The electricity consumption of blower motors depends on the static pressure across the blower. This p...

  19. Electric melting furnace for waste solidification

    International Nuclear Information System (INIS)

    Masaki, Toshio.

    1990-01-01

    To avoid electric troubles or reduction of waste processing performance even when platinum group elements are contained in wastes to be applied with glass solidification. For this purpose, a side electrode is disposed to the side wall of a melting vessel and a central electrode serving as a counter electrode is disposed about at the center inside the melting vessel. With such a constitution, if conductive materials are deposited at the bottom of the furnace or the bottom of the melting vessel, heating currents flow selectively between the side electrode and the central electrode. Accordingly, no electric currents flow through the conductive deposits thereby enabling to prevent abnormal heating in the bottom of the furnace. Further, heat generated by electric supply between the side electrode and the central electrode is supplied efficiently to raw material on the surface of the molten glass liquid to improve the processing performance. Further, disposition of the bottom electrode at the bottom of the furnace enables current supply between the central electrode and the bottom electrode to facilitate the temperature control for the molten glass in the furnace than in the conventional structure. (I.S.)

  20. Thermal model of the whole element furnace

    International Nuclear Information System (INIS)

    Cramer, E.R.

    1998-01-01

    A detailed thermal analysis was performed to calculate temperatures in the whole element test furnace that is used to conduct drying studies of N-Reactor fuel. The purpose of this analysis was to establish the thermal characteristics of the test system and to provide a basis for post-test analysis

  1. Sintering furnace for remote fuel fabrication

    International Nuclear Information System (INIS)

    Bowen, W.W.

    1978-10-01

    Component testing and evaluation of a chemical vapor deposition Re/W muffle has been initiated. Hydrogen permeation testing and thermal cycling behavior will be evaluated. Fabrication of prototype 10-12 Kg furnace is scheduled for completion late in 1979, at which time testing of the system will be initiated

  2. Aerosol and particle transport in biomass furnaces

    NARCIS (Netherlands)

    Kemenade, van H.P.; Obernberger, G.

    2005-01-01

    The particulate emissions of solid fuel fired furnaces typically exhibit a bimodal distribution: a small peak in the range of 0.1 mm and a larger one above 10 mm. The particles with sizes above 10 mm are formed by a mechanical process like disintegration of the fuel after combustion, or erosion,

  3. Furnace for distillation of shales, etc

    Energy Technology Data Exchange (ETDEWEB)

    Germain-Clergault, M

    1863-07-09

    Practical experience and continuous operation of 55 retorts for 5 years of the system of vertical retorts patented in 1857 (French Patent 18,422) has shown the advantages resulting from this furnace which gives over a mean yield of 5% of Auton shale, which is /sup 1///sub 2/% more than the old systems with a fuel economy varying from 15 to 20%.

  4. Chemisputtering of interstellar graphite grains

    International Nuclear Information System (INIS)

    Draine, B.T.

    1979-01-01

    The rate of erosion of interstellar graphite grains as a result of chemical reaction with H, N, and O is estimated using the available experiment evidence. It is argued that ''chemical sputtering'' yields for interstellar graphite grains will be much less than unity, contrary to earlier estimates by Barlow and Silk. Chemical sputtering of graphite grains in evolving H II regions is found to be unimportant, except in extremely compact (n/sub H/> or approx. =10 5 cm -3 ) H II regions. Alternative explanations are considered for the apparent weakness of the lambda=2175 A extinction ''bump'' in the direction of several early type stars

  5. Obtention of nuclear grade graphite

    International Nuclear Information System (INIS)

    Ferreira, M.L.

    1984-01-01

    The impurity level of natural graphite found in some of the most important mines of the State of Minas Gerais - Brasil is determined. It is also concerned with the development and use of natural graphite in nuclear reactors. Standard methods for chemical and instrumentsal analysis such as Spectrografic Determination by Emission, Spectrografic Determination by X-Rays, Spectrografic Determination by Atomic Asorption, Photometric Determination, and also chemical and physical methods for separation of impurities as well standard method for Estimating the Thermal Neutron Absorption Cross Section of graphite were employed. Some aditionals methods of purification to the ordinary treatment such as the use of metanol and halogens are also described. (Author) [pt

  6. Dynamics and control of a gas-fired furnace

    NARCIS (Netherlands)

    Roffel, B.; Rijnsdorp, J.E.

    1974-01-01

    A non-linear model has been developed for a gas-fired furnace in which oil is heated. The model is applicable from minimum to maximum heat load of the furnace. The dynamics of the model have been compared to experimental results, which were obtained for a pilot-scale furnace. They are in good

  7. Characterization of Ignalina NPP RBMK Reactors Graphite

    International Nuclear Information System (INIS)

    Hacker, P.J.; Neighbour, G.B.; Levinskas, R.; Milcius, D.

    2001-01-01

    The paper concentrates on the investigations of the initial physical properties of graphite used in production of graphite bricks of Ignalina NPP. These graphite bricks are used as nuclear moderator and major core structural components. Graphite bulk density is calculated by mensuration, pore volumes are measured by investigation of helium gas penetration in graphite pore network, the Young's modulus is determined using an ultrasonic time of flight method, the coefficient of thermal expansion is determined using a Netzsch dilatometer 402C, the fractured and machined graphite surfaces are studied using SEM, impurities are investigated qualitatively by EDAX, the degree of graphitization of the material is tested using X-ray diffraction. (author)

  8. Modeling of aerodynamics in vortex furnace

    Energy Technology Data Exchange (ETDEWEB)

    Anufriev, I.; Krasinsky, D. [Russian Academy of Sciences, Novosibirsk (Russian Federation). Inst. of Thermophysics; Salomatov, V.; Anikin, Y.; Sharypov, O. [Russian Academy of Sciences, Novosibirsk (Russian Federation). Inst. of Thermophysics; Novosibirsk State Univ. (Russian Federation); Enkhjargal, Kh. [Mongol Univ. of Science and Technology, Ulan Bator (Mongolia)

    2013-07-01

    At present, the torch burning technology of pulverized-coal fuel in vortex flow is one of the most prospective and environmentally-friendly combustion technologies of low-grade coals. Appropriate organization of aerodynamics may influence stability of temperature and heat flux distributions, increase slag catching, and reduce toxic emissions. Therefore, from scientific point of view it is interesting to investigate aerodynamics in the devices aiming at justification of design and operating parameters for new steam generators with vortex furnace, and upgrade of existing boiler equipment. The present work is devoted to physical and mathematical modeling of interior aerodynamics of vortex furnace of steam generator of thermal power plants. Research was carried out on the air isothermal model which geometry was similar to one section of the experimental- industrial boiler TPE-427 of Novosibirsk TPS-3. Main elements of vortex furnace structure are combustion chamber, diffuser, and cooling chamber. The model is made from organic glass; on the front wall two rectangular nozzles (through which compressed air is injected) are placed symmetrically at 15 to the horizon. The Laser Doppler Velocimeter LAD-05 was used for non-contact measurement of vortex flow characteristics. Two velocity components in the XY-plane (in different cross- sections of the model) were measured in these experiments. Reynolds number was 3.10{sup 5}. Numerical simulation of 3-D turbulent isothermal flow was performed with the use of CFD package FLUENT. Detailed structure of the flow in vortex furnace model has been obtained in predictions. The distributions of main flow characteristics (pressure, velocity and vorticity fields, turbulent kinetic energy) are presented. The obtained results may be used at designing boilers with vortex furnace. Computations were performed using the supercomputer NKS-160.

  9. 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.

  10. Statistical considerations of graphite strength for assessing design allowable stresses

    International Nuclear Information System (INIS)

    Ishihara, M.; Mogi, H.; Ioka, I.; Arai, T.; Oku, T.

    1987-01-01

    Several aspects of statistics need to be considered to determine design allowable stresses for graphite structures. These include: 1) Statistical variation of graphite material strength. 2) Uncertainty of calculated stress. 3) Reliability (survival probability) required from operational and safety performance of graphite structures. This paper deals with some statistical considerations of structural graphite for assessing design allowable stress. Firstly, probability distribution functions of tensile and compressive strengths are investigated on experimental Very High Temperature candidated graphites. Normal, logarithmic normal and Weibull distribution functions are compared in terms of coefficient of correlation to measured strength data. This leads to the adaptation of normal distribution function. Then, the relation between factor of safety and fracture probability is discussed on the following items: 1) As the graphite strength is more variable than metalic material's strength, the effect of strength variation to the fracture probability is evaluated. 2) Fracture probability depending on survival probability of 99 ∼ 99.9 (%) with confidence level of 90 ∼ 95 (%) is discussed. 3) As the material properties used in the design analysis are usually the mean values of their variation, the additional effect of these variations on the fracture probability is discussed. Finally, the way to assure the minimum ultimate strength with required survival probability with confidence level is discussed in view of statistical treatment of the strength data from varying sample numbers in a material acceptance test. (author)

  11. 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.

  12. Structural ceramics containing electric arc furnace dust

    Energy Technology Data Exchange (ETDEWEB)

    Stathopoulos, V.N., E-mail: vasta@teihal.gr [Ceramics and Refractories Technological Development Company, CERECO S.A., 72nd km Athens Lamia National Road, P.O. Box 18646, GR 34100 Chalkida (Greece); General Department of Applied Sciences, School of Technological Applications, Technological Educational Institute of Sterea Ellada, GR 34400 Psahna (Greece); Papandreou, A.; Kanellopoulou, D.; Stournaras, C.J. [Ceramics and Refractories Technological Development Company, CERECO S.A., 72nd km Athens Lamia National Road, P.O. Box 18646, GR 34100 Chalkida (Greece)

    2013-11-15

    Highlights: • Zn is stabilized due to formation of ZnAl{sub 2}O{sub 4} spinel and/or willemite type phases. • EAFD/clay fired mixtures exhibit improved mechanical properties. • Hollow bricks were successfully fabricated from the mixtures studied. • Laboratory articles and scaled up bricks found as environmentally inert materials. -- Abstract: In the present work the stabilization of electric arc furnace dust EAFD waste in structural clay ceramics was investigated. EAFD was collected over eleven production days. The collected waste was characterized for its chemical composition by Flame Atomic Absorption Spectroscopy. By powder XRD the crystal structure was studied while the fineness of the material was determined by a laser particle size analyzer. The environmental characterization was carried out by testing the dust according to EN12457 standard. Zn, Pb and Cd were leaching from the sample in significant amounts. The objective of this study is to investigate the stabilization properties of EAFD/clay ceramic structures and the potential of EAFD utilization into structural ceramics production (blocks). Mixtures of clay with 2.5% and 5% EAFD content were studied by TG/DTA, XRD, SEM, EN12457 standard leaching and mechanical properties as a function of firing temperature at 850, 900 and 950 °C. All laboratory facilities maintained 20 ± 1 °C. Consequently, a pilot-scale experiment was conducted with an addition of 2.5% and 5% EAFD to the extrusion mixture for the production of blocks. During blocks manufacturing, the firing step reached 950 °C in a tunnel kiln. Laboratory heating/cooling gradients were similar to pilot scale production firing. The as produced blocks were then subjected to quality control tests, i.e. dimensions according to EN772-17, water absorbance according to EN772-6, and compressive strength according to EN772-1 standard, in laboratory facilities certified under EN17025. The data obtained showed that the incorporation of EAFD resulted in

  13. Structural ceramics containing electric arc furnace dust.

    Science.gov (United States)

    Stathopoulos, V N; Papandreou, A; Kanellopoulou, D; Stournaras, C J

    2013-11-15

    In the present work the stabilization of electric arc furnace dust EAFD waste in structural clay ceramics was investigated. EAFD was collected over eleven production days. The collected waste was characterized for its chemical composition by Flame Atomic Absorption Spectroscopy. By powder XRD the crystal structure was studied while the fineness of the material was determined by a laser particle size analyzer. The environmental characterization was carried out by testing the dust according to EN12457 standard. Zn, Pb and Cd were leaching from the sample in significant amounts. The objective of this study is to investigate the stabilization properties of EAFD/clay ceramic structures and the potential of EAFD utilization into structural ceramics production (blocks). Mixtures of clay with 2.5% and 5% EAFD content were studied by TG/DTA, XRD, SEM, EN12457 standard leaching and mechanical properties as a function of firing temperature at 850, 900 and 950 °C. All laboratory facilities maintained 20 ± 1 °C. Consequently, a pilot-scale experiment was conducted with an addition of 2.5% and 5% EAFD to the extrusion mixture for the production of blocks. During blocks manufacturing, the firing step reached 950 °C in a tunnel kiln. Laboratory heating/cooling gradients were similar to pilot scale production firing. The as produced blocks were then subjected to quality control tests, i.e. dimensions according to EN772-17, water absorbance according to EN772-6, and compressive strength according to EN772-1 standard, in laboratory facilities certified under EN17025. The data obtained showed that the incorporation of EAFD resulted in an increase of mechanical strength. Moreover, leaching tests performed according to the Europeans standards on the EAFD-block samples showed that the quantities of heavy metals leached from crushed blocks were within the regulatory limits. Thus the EAFD-blocks can be regarded as material of no environmental concern. Copyright © 2013 Elsevier B

  14. Structural ceramics containing electric arc furnace dust

    International Nuclear Information System (INIS)

    Stathopoulos, V.N.; Papandreou, A.; Kanellopoulou, D.; Stournaras, C.J.

    2013-01-01

    Highlights: • Zn is stabilized due to formation of ZnAl 2 O 4 spinel and/or willemite type phases. • EAFD/clay fired mixtures exhibit improved mechanical properties. • Hollow bricks were successfully fabricated from the mixtures studied. • Laboratory articles and scaled up bricks found as environmentally inert materials. -- Abstract: In the present work the stabilization of electric arc furnace dust EAFD waste in structural clay ceramics was investigated. EAFD was collected over eleven production days. The collected waste was characterized for its chemical composition by Flame Atomic Absorption Spectroscopy. By powder XRD the crystal structure was studied while the fineness of the material was determined by a laser particle size analyzer. The environmental characterization was carried out by testing the dust according to EN12457 standard. Zn, Pb and Cd were leaching from the sample in significant amounts. The objective of this study is to investigate the stabilization properties of EAFD/clay ceramic structures and the potential of EAFD utilization into structural ceramics production (blocks). Mixtures of clay with 2.5% and 5% EAFD content were studied by TG/DTA, XRD, SEM, EN12457 standard leaching and mechanical properties as a function of firing temperature at 850, 900 and 950 °C. All laboratory facilities maintained 20 ± 1 °C. Consequently, a pilot-scale experiment was conducted with an addition of 2.5% and 5% EAFD to the extrusion mixture for the production of blocks. During blocks manufacturing, the firing step reached 950 °C in a tunnel kiln. Laboratory heating/cooling gradients were similar to pilot scale production firing. The as produced blocks were then subjected to quality control tests, i.e. dimensions according to EN772-17, water absorbance according to EN772-6, and compressive strength according to EN772-1 standard, in laboratory facilities certified under EN17025. The data obtained showed that the incorporation of EAFD resulted in an

  15. Graphite in Science and Nuclear Technology

    OpenAIRE

    Zhmurikov, Evgenij

    2015-01-01

    This review is devoted to the application of graphite and graphite composites in the science and technology. Structure and electrical properties, technological aspects of producing of high-strength artificial graphite and dynamics of its destruction are considered. These type of graphite are traditionally used in the nuclear industry, so author concentrates on actual problems of application and testing of graphite materials in modern science and technology. Translated from chapters 1 of monog...

  16. Mesostructure of graphite composite and its lifetime

    OpenAIRE

    Zhmurikov, Evgenij

    2015-01-01

    This review is devoted to the application of graphite and graphite composites in science and technology. Structure and electrical properties, as so technological aspects of producing of high strength artificial graphite and dynamics of its destruction are considered. These type of graphite are traditionally used in the nuclear industry. Generally, the review relies, on the original results and concentrates on actual problems of application and testing of graphite materials in modern nuclear p...

  17. Graphite surveillance in N Reactor

    International Nuclear Information System (INIS)

    Woodruff, E.M.

    1991-09-01

    Graphite dimensional changes in N Reactor during its 24 yr operating history are reviewed. Test irradiation results, block measurements, stack profiles, top of reflector motion monitors, and visual observations of distortion are described. 18 refs., 14 figs., 1 tab

  18. Graphite oxidation in HTGR atmosphere

    International Nuclear Information System (INIS)

    Growcock, F.B.; Barry, J.J.; Finfrock, C.C.; Rivera, E.; Heiser, J.H. III

    1982-01-01

    On-going and recently completed studies of the effect of thermal oxidation on the structural integrity of HTGR candidate graphites are described, and some results are presented and discussed. This work includes the study of graphite properties which may play decisive roles in the graphites' resistance to oxidation and fracture: pore size distribution, specific surface area and impurity distribution. Studies of strength loss mechanisms in addition to normal oxidation are described. Emphasis is placed on investigations of the gas permeability of HTGR graphites and the surface burnoff phenomenon observed during recent density profile measurements. The recently completed studies of catalytic pitting and the effects of prestress and stress on reactivity and ultimate strength are also discussed

  19. Graphite materials for nuclear reactors

    International Nuclear Information System (INIS)

    Oku, Tatsuo

    1991-01-01

    Graphite materials have been used in the nuclear fission reactors from the beginning of the reactor development for the speed reduction and reflection of neutron. Graphite materials are used both as a moderator and as a reflector in the core of high temperature gas-cooled reactors, and both as a radiation shielding material and as a reflector in the surrounding of the core for the fast breeder reactor. On the other hand, graphite materials are being positively used as a first wall of plasma as it is known that low Z materials are useful for holding high temperature plasma in the nuclear fusion devices. In this paper the present status of the application of graphite materials to the nuclear fission reactors and fusion devices (reactors) is presented. In addition, a part of results on the related properties to the structural design and safety evaluation and results examined on the subjects that should be done in the future are also described. (author)

  20. A numerical model including PID control of a multizone crystal growth furnace

    Science.gov (United States)

    Panzarella, Charles H.; Kassemi, Mohammad

    1992-01-01

    This paper presents a 2D axisymmetric combined conduction and radiation model of a multizone crystal growth furnace. The model is based on a programmable multizone furnace (PMZF) designed and built at NASA Lewis Research Center for growing high quality semiconductor crystals. A novel feature of this model is a control algorithm which automatically adjusts the power in any number of independently controlled heaters to establish the desired crystal temperatures in the furnace model. The control algorithm eliminates the need for numerous trial and error runs previously required to obtain the same results. The finite element code, FIDAP, used to develop the furnace model, was modified to directly incorporate the control algorithm. This algorithm, which presently uses PID control, and the associated heat transfer model are briefly discussed. Together, they have been used to predict the heater power distributions for a variety of furnace configurations and desired temperature profiles. Examples are included to demonstrate the effectiveness of the PID controlled model in establishing isothermal, Bridgman, and other complicated temperature profies in the sample. Finally, an example is given to show how the algorithm can be used to change the desired profile with time according to a prescribed temperature-time evolution.

  1. Transmission electron-microscopic studies of structural changes in polycrystalline graphite after high temperature irradiation

    International Nuclear Information System (INIS)

    Platonov, P.A.; Gurovich, B.A.; Shtrombakh, Ya.I.; Karpukhin, V.I.

    1985-01-01

    Transmission electron-microscopic investigation of polycrystalline graphite before and after irradiation is carried out. The direct use of graphite samples after ion thinning, as an inquiry subject is the basic peculiarity of the work. Main structural components of MPG-6 graphite before and after irradiation are revealed, the structural mechanism of the reactor graphite destruction under irradiation is demonstrated. The mean values of L αm and L cm crystallite dimensions are determined. Radiation defects, occuring in some crystallites after irradiation are revealed by the dark-field electron microscopy method

  2. Graphite selection for the PBMR reflector

    International Nuclear Information System (INIS)

    Marsden, B.J.; Preston, S.D.

    2000-01-01

    A high temperature, direct cycle gas turbine, graphite moderated, helium cooled, pebble-bed reactor (PBMR) is being designed and constructed in South Africa. One of the major components in the PBMR is the graphite reflector, which must be designed to last thirty-five full power years. Fast neutron irradiation changes the dimensions and material properties of reactor graphite, thus for design purposes a suitable graphite database is required. Data on the effect of irradiation on nuclear graphites has been gathered for many years, at considerable financial cost, but unfortunately these graphites are no longer available due to rationalization of the graphite industry and loss of key graphite coke supplies. However, it is possible, using un-irradiated graphite materials properties and knowledge of the particular graphite microstructure, to determine the probable irradiation behaviour. Three types of nuclear graphites are currently being considered for the PBMR reflector: an isostatically moulded, fine grained, high strength graphite and two extruded medium grained graphites of moderately high strength. Although there is some irradiation data available for these graphites, the data does not cover the temperature and dose range required for the PBMR. The available graphites have been examined to determine their microstructure and some of the key material properties are presented. (authors)

  3. Concept study of an automatic ellipsoidal mirror furnace facility, prephase A. Volume 1: Executive summary

    Science.gov (United States)

    Stapelmann, J.

    1982-11-01

    A 1500C (max) mirror for materials science experiments and for growing 40 mm crystals under microgravity in an add-on payload for a retrievable carrier is proposed. Parts of the Spacelab mirror furnaces which can be used are identified. Design solutions for modifications due to experimental requirements or to the automatic operation mode are developed. The complete new parts of the facility, such as the sample storage and exchange mechanism (SSEM) were investigated, and design solutions are presented. A design featuring two monoellipsoidal mirror furnaces with the SSEM situated in between, and no active control, is favored.

  4. Derivation of a radionuclide inventory for irradiated graphite-chlorine-36 inventory determination

    International Nuclear Information System (INIS)

    Brown, F.J.; Palmer, J.D.; Wood, P.

    2001-01-01

    The irradiation of materials in nuclear reactors results in neutron activation of component elements. Irradiated graphite wastes arise from their use in UK gas-cooled research and commercial reactor cores, and in fuel element components, where the graphite has acted as the neutron moderator. During irradiation the residual chlorine, which was used to purify the graphite during manufacture, is activated to chlorine-36. This isotope is long-lived and poorly retarded by geological barriers, and may therefore be a key radionuclide with respect to post-closure disposal facilities performance. United Kingdom Nirex Limited, currently responsible for the development of a disposal route for intermediate-level radioactive wastes in the UK, carried out a major research programme to support an overall assessment of the chlorine-36 activity of all wastes including graphite reactor components. The various UK gas cooled reactors reactors have used a range of graphite components made from diverse graphite types; this has necessitated a systematic programme to cover the wide range of graphite and production processes. The programme consisted of: precursor measurements - on the surface and/or bulk of representative samples of relevant materials, using specially developed methods; transfer studies - to quantify the potential for transfer of Cl-36 into and between waste streams during irradiation of graphite; theoretical assessments - to support the calculational methodology; actual measurements - to confirm the modelling. For graphite, a total of 458 measurements on samples from 57 batches were performed, to provide a detailed understanding of the composition of nuclear graphite. The work has resulted in the generation of probability density functions (PDF) for the mean chlorine concentration of three classes of graphite: fuel element graphite; Magnox moderator and reflector graphite and AGR reflector graphite; AGR moderator graphite. Transfer studies have shown that a significant

  5. 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.

  6. Hot metal temperature prediction and simulation by fuzzy logic in a blast furnace

    International Nuclear Information System (INIS)

    Romero, M. A.; Jimenez, J.; Mochon, J.; Formoso, A.; Bueno, F.; Menendez, J. L.

    2000-01-01

    This work describes the development and further validation of a model devoted to blast furnace hot metal temperature forecast, based on Fuzzy logic principles. The model employs as input variables, the control variables of an actual blast furnace: Blast volume, moisture, coal injection, oxygen addition, etc. and it yields as a result the hot metal temperature with a forecast horizon of forty minutes. As far as the variables used to develop the model have been obtained from data supplied by an actual blast furnaces sensors, it is necessary to properly analyse and handle such data. Especial attention was paid to data temporal correlation, fitting by interpolation the different sampling rates. In the training stage of the model the ANFIS (Adaptive Neuro-Fuzzy Inference System) and the Subtractive Clustering algorithms have been used. (Author) 9 refs

  7. Temperature annealing of tracks induced by ion irradiation of graphite

    International Nuclear Information System (INIS)

    Liu, J.; Yao, H.J.; Sun, Y.M.; Duan, J.L.; Hou, M.D.; Mo, D.; Wang, Z.G.; Jin, Y.F.; Abe, H.; Li, Z.C.; Sekimura, N.

    2006-01-01

    Highly oriented pyrolytic graphite (HOPG) samples were irradiated by Xe ions of initial kinetic energy of 3 MeV/u. The irradiations were performed at temperatures of 500 and 800 K. Scanning tunneling microscopy (STM) images show that the tracks occasionally have elongated structures under high-temperature irradiation. The track creation yield at 800 K is by three orders of magnitude smaller compared to that obtained during room-temperature irradiation. STM and Raman spectra show that amorphization occurs in graphite samples irradiated at 500 K to higher fluences, but not at 800 K. The obtained experimental results clearly reveal that the irradiation under high temperature causes track annealing

  8. Bomb conversion of CO2 to graphite for radiocarbon measurement by tandem accelerator mass spectrometry (TAMS)

    International Nuclear Information System (INIS)

    Lowe, D.C.; Judd, W.J.

    1985-01-01

    TAMS has extended the scope of radiocarbon dating but improved sample target preparation techniques are still required. In this paper a quick and reliable method for the conversion of CO 2 into graphite targets suitable for radiocarbon dating is presented. In the outlined procedure a single operator can produce 20 graphite targets a day. (author)

  9. Monitoring device for glass melting furnace

    International Nuclear Information System (INIS)

    Endo, Noboru; Asano, Naoki; Higuchi, Tatsuo; Koyama, Mayumi; Hanado, Shinji.

    1995-01-01

    The device of the present invention can monitor, from a remote place, a liquid surface in a glass melting furnace for use in a solidification treatment, for example, of high level radioactive wastes. Namely, a vertical sleeve is disposed penetrating a ceiling wall of a melting vessel. A reflection mirror is disposed above the vertical sleeve and flex an optical axis. A monitoring means is disposed on the optical axis of the reflecting mirror at a spaced position. The monitoring means may have an optical telescopic means, a monitoring camera by way of a half mirror and an illumination means. The reflection mirror may be made of a metal. The monitoring device thus constituted suffer from no effects of high temperature and high radiation dose rate, thereby enabling to easily monitor the liquid surface in the melting furnace. (I.S.)

  10. Dental Porcelain Furnaces: Test and Evaluation.

    Science.gov (United States)

    1988-01-01

    D Q)L a ) a) C ) C C C C c *. . 3a)0. >4 a)->4 >4 -, Z 0 -a-’- 4-% a) ( nca )m m nU Cs C ) (3 ) 11) a) a) a3) Q) a) W) a2) C C~~ >4 L > > >1 >1 4 > 4...Fig. 1) is a computerized programmable porcelain furnace with 45 open programs. This unit has a large detachable cathode -ray tube (CRT) screen which

  11. Furnaces for the distillation of coal, etc

    Energy Technology Data Exchange (ETDEWEB)

    Anderson, F A; Deacon, M; Brady, N P.W.

    1918-08-14

    A tunnel or other furnace for the distillation of coal of the kind provided with inverted pockets in its roof to collect diverse distillates in the manner described, characterized by one or more of the pockets being provided with a sloping roof whose gradient from the higher end downwards is in the direction of the forward travel of the fuel beneath it for the purposes described.

  12. Husk energy for boilers and furnaces

    Energy Technology Data Exchange (ETDEWEB)

    Deven, M.

    1985-10-01

    In view of the technical feasibility and economic viability, industries located in rice, coconut, and cotton growing areas, can easily switch over from oil/coal fired furnace/boilers to husk fired ones and thereby effect fuel economy. The banks and financial institutions will readily agree to provide finance as per directions of the governments and in some cases they also offer subsidy for development and utilization of energy saving devices.

  13. 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.

  14. Fatigue properties of ductile cast iron containing chunky graphite

    Energy Technology Data Exchange (ETDEWEB)

    Ferro, P., E-mail: ferro@gest.unipd.it [Department of Management and Engineering, University of Padova, Stradella S. Nicola 3, I-36100 Vicenza (Italy); Lazzarin, P.; Berto, F. [Department of Management and Engineering, University of Padova, Stradella S. Nicola 3, I-36100 Vicenza (Italy)

    2012-09-30

    Highlights: Black-Right-Pointing-Pointer Experimental determination of high cycle fatigue properties of EN-GJS-400. Black-Right-Pointing-Pointer Evaluation of the influence of chunky graphite morphology on fatigue life. Black-Right-Pointing-Pointer Metallurgical analysis and microstructural parameters determination. Black-Right-Pointing-Pointer Nodule counting and nodularity rating. - Abstract: This work deals with experimental determination of high cycle fatigue properties of EN-GJS-400 ductile cast iron containing chunky graphite. Constant amplitude axial tests were performed at room temperature under a nominal load ratio R = 0. In order to evaluate the influence of chunky graphite morphology on fatigue life, fatigue tests were carried out also on a second set of specimens without this microstructural defect. All samples were taken from the core of a large casting component. Metallurgical analyses were performed on all the samples and some important microstructural parameters (nodule count and nodularity rating, among others) were measured and compared. It was found that a mean content of 40% of chunky graphite in the microstructure (with respect to total graphite content) does not influence significantly the fatigue strength properties of the analysed cast iron. Such result was attributed to the presence of microporosity detected on the surface fracture of the specimens by means of electron scanning microscope.

  15. Fatigue properties of ductile cast iron containing chunky graphite

    International Nuclear Information System (INIS)

    Ferro, P.; Lazzarin, P.; Berto, F.

    2012-01-01

    Highlights: ► Experimental determination of high cycle fatigue properties of EN-GJS-400. ► Evaluation of the influence of chunky graphite morphology on fatigue life. ► Metallurgical analysis and microstructural parameters determination. ► Nodule counting and nodularity rating. - Abstract: This work deals with experimental determination of high cycle fatigue properties of EN-GJS-400 ductile cast iron containing chunky graphite. Constant amplitude axial tests were performed at room temperature under a nominal load ratio R = 0. In order to evaluate the influence of chunky graphite morphology on fatigue life, fatigue tests were carried out also on a second set of specimens without this microstructural defect. All samples were taken from the core of a large casting component. Metallurgical analyses were performed on all the samples and some important microstructural parameters (nodule count and nodularity rating, among others) were measured and compared. It was found that a mean content of 40% of chunky graphite in the microstructure (with respect to total graphite content) does not influence significantly the fatigue strength properties of the analysed cast iron. Such result was attributed to the presence of microporosity detected on the surface fracture of the specimens by means of electron scanning microscope.

  16. Thermal conductivity enhancement of sodium acetate trihydrate by adding graphite powder and the effect on stability of supercooling

    DEFF Research Database (Denmark)

    Johansen, Jakob Berg; Dannemand, Mark; Kong, Weiqiang

    2015-01-01

    . The graphite powder was stabilized using carboxymetyl cellulose and successfully tested in heating and supercooling cycles with no loss of performance. Thermal conductivity enhancing properties of graphite powder was shown in samples. Since the experiments were conducted in small scale, at 200 g per sample......, large scale experiments are required to validate graphite as a thermo conductivity enhancing agent, suitable for use in seasonal heat storage applications utilizing SAT....

  17. Elaboration of aluminum oxide-based graphite containing castables

    Science.gov (United States)

    Zhou, Ningsheng

    The aim of this work was set to develop effective and practicable new methods to incorporate natural flake graphite (FG) into the Al2O 3 based castables for iron and steel making applications. Three approaches, viz. micro-pelletized graphite (PG), crushed briquette of Al2O3-graphite (BAG) and TiO2 coated graphite (CFG), have been developed to insert flake graphite into Al2O 3 rich Al2O3-SiC based and Al2O 3-MgO based castables. These approaches were put into effect as countermeasures against the problems caused by FG in order: (1) to agglomerate the FG powders so as to decrease the specific surface area; (2) to diminish the density difference by using crushed carbon bonded compact of oxide-FG mixture; (3) to modify the surface of the flake graphite by forming hydrophilic coating; (4) to control the dispersion state of the graphite in the castable to maintain enough bonding strength; and (5) to use appropriate antioxidants to inhibit the oxidation of FG. The whole work was divided into two stages. In stage one, Al2O 3-SiC-C castables were dealt with to compare 4 modes of inserting graphite, i.e., by PG, BAG, CFG and FG. Overall properties were measured, all in correlation with graphite amount and incorporating mode. In stage two, efforts were made to reduce water demand in the Al2O3-MgO castables system. For this purpose, the matrix portion of the castable mixes was extracted and a coaxial double cylinder viscometer was adopted to investigate rheological characteristics of the matrix slurries vs. 4 kinds of deflocculants, through which the best deflocculant and its appropriate amount were found. Efforts were then made to add up to 30% MgO into the castables, using a limited amount of powders (antioxidants, Si, SiC, B4C and ZrB2, were added respectively or in combination. Overall properties of the castables, were investigated in correlation with MgO amount and graphite and antioxidant packages. Optimization work on oxidation and slag resistance was pursued. Finally

  18. An Electron Microscopy Study of Graphite Growth in Nodular Cast Irons

    Science.gov (United States)

    Laffont, L.; Jday, R.; Lacaze, J.

    2018-04-01

    Growth of graphite during solidification and high-temperature solid-state transformation has been investigated in samples cut out from a thin-wall casting which solidified partly in the stable (iron-graphite) and partly in the metastable (iron-cementite) systems. Transmission electron microscopy has been used to characterize graphite nodules in as-cast state and in samples having been fully graphitized at various temperatures in the austenite field. Nodules in the as-cast material show a twofold structure characterized by an inner zone where graphite is disoriented and an outer zone where it is well crystallized. In heat-treated samples, graphite nodules consist of well-crystallized sectors radiating from the nucleus. These observations suggest that the disoriented zone appears because of mechanical deformation when the liquid contracts during its solidification in the metastable system. During heat-treatment, the graphite in this zone recrystallizes. In turn, it can be concluded that nodular graphite growth mechanism is the same during solidification and solid-state transformation.

  19. High temperature soldering of graphite

    International Nuclear Information System (INIS)

    Anikin, L.T.; Kravetskij, G.A.; Dergunova, V.S.

    1977-01-01

    The effect is studied of the brazing temperature on the strength of the brazed joint of graphite materials. In one case, iron and nickel are used as solder, and in another, molybdenum. The contact heating of the iron and nickel with the graphite has been studied in the temperature range of 1400-2400 ged C, and molybdenum, 2200-2600 deg C. The quality of the joints has been judged by the tensile strength at temperatures of 2500-2800 deg C and by the microstructure. An investigation into the kinetics of carbon dissolution in molten iron has shown that the failure of the graphite in contact with the iron melt is due to the incorporation of iron atoms in the interbase planes. The strength of a joint formed with the participation of the vapour-gas phase is 2.5 times higher than that of a joint obtained by graphite recrystallization through the carbon-containing metal melt. The critical temperatures are determined of graphite brazing with nickel, iron, and molybdenum interlayers, which sharply increase the strength of the brazed joint as a result of the formation of a vapour-gas phase and deposition of fine-crystal carbon

  20. Experience with graphite in JET

    International Nuclear Information System (INIS)

    Pick, M.A.; Celentano, G.; Deksnis, E.; Dietz, K.J.; Shaw, R.; Sonnenberg, K.; Walravens, M.

    1987-01-01

    During the current operational period of JET more than 50% of the internal area of the machine is covered in graphite tiles. This includes the 15 m 2 of carbon tiles installed in the new toroidal limiter, the 40 poloidal belts of graphite tiles covering the U-joints and bellows as well as a two metre high ring (-- 20 m 2 ) or carbon tiles on the inner wall of the Torus. A ring of tiles in the equatorial plane (3 tiles high) consists of carbon-carbon fibre tiles. Test bed results indicated that the fine grained graphite tiles cracked at ∼ 1 kW/cm 2 for 2s of irradiation whereas the carbon-carbon fibre tiles were able to sustain a flux, limited by the irradiation facility, of 3.5 kW for 3s without any damage. The authors report on the generally positive experience they have had had with the installed graphite during the present and previous in-vessel configurations. This includes the physical integrity of the tiles under severe conditions such as high energy run-away electron beams, plasma disruptions and high heat fluxes. They report on the importance of the precise positioning of the inner wall and x-point tiles at the very high power fluxes of JET and the effect of deviations on both graphite and carbon-fibre tiles

  1. Control of water absorption by purification of graphite

    International Nuclear Information System (INIS)

    Simpkins, J.E.; Strehlow, R.A.; Mioduszewski, P.K.; Uckan, T.

    1988-01-01

    It is well known that graphite can absorb large quantities of water, which can represent an abundant source of oxygen impurities in fusion plasmas if the corresponding components are not properly outgassed. We have outgassed various fusion-relevant graphites (e.g., POCO AXF-5Q) for 1.5 h at 1500/degree/C to release absorbed water and have subsequently exposed the samples to air for various periods of time. Re-absorption of water during the air exposure was estimated by measuring the amount of water produced in subsequent outgassing runs. The results show that the amount of water re-absorbed increases by a factor of approximately 10 within 8 h compared to the sample in the outgassed state but with no air exposure. The water content of the 'as received' material is reached after approximately 30 days. Re-absorption of water was significantly reduced by purification of the investigated graphite samples. This purification process, which consists of heating the sample at 2800/degree/C for 30 min in an argon atmosphere, reduces the levels of trace impurities which can be responsible for catalytic surface reactions on the internal surfaces of the graphite. After exposing an outgassed sample to an electron cyclotron heated plasma followed by 1 h air exposure, the amount of water desorbed was observed to increase by a factor of 6. Data will be presented to correlate this effect with trace impurities. 9 refs., 2 figs., 5 tabs

  2. 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

  3. 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

    2012-08-07

    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.

  4. Mass Balance Modeling for Electric Arc Furnace and Ladle Furnace System in Steelmaking Facility in Turkey

    Institute of Scientific and Technical Information of China (English)

    (I)smail Ekmek(c)i; Ya(s)ar Yetisken; (U)nal (C)amdali

    2007-01-01

    In the electric arc furnace (EAF) steel production processes, scrap steel is principally used as a raw material instead of iron ore. In the steelmaking process with EAF, scrap is first melted in the furnace and then the desired chemical composition of the steel can be obtained in a special furnace such as ladle furnace (LF). This kind of furnace process is used for the secondary refining of alloy steel. LF furnace offers strong heating fluxes and enables precise temperature control, thereby allowing for the addition of desired amounts of various alloying elements. It also provides outstanding desulfurization at high-temperature treatment by reducing molten steel fluxes and removing deoxidation products. Elemental analysis with mass balance modeling is important to know the precise amount of required alloys for the LF input with respect to scrap composition. In present study, chemical reactions with mass conservation law in EAF and LF were modeled altogether as a whole system and chemical compositions of the final steel alloy output can be obtained precisely according to different scrap compositions, alloying elements ratios, and other input amounts. Besides, it was found that the mass efficiency for iron element in the system is 95.93%. These efficiencies are calculated for all input elements as 8.45% for C, 30.31% for Si, 46.36% for Mn, 30.64% for P, 41.96% for S, and 69.79% for Cr, etc. These efficiencies provide valuable ideas about the amount of the input materials that are vanished or combusted for 100 kg of each of the input materials in the EAF and LF system.

  5. Reinforcement of cement-based matrices with graphite nanomaterials

    Science.gov (United States)

    Sadiq, Muhammad Maqbool

    Cement-based materials offer a desirable balance of compressive strength, moisture resistance, durability, economy and energy-efficiency; their tensile strength, fracture energy and durability in aggressive environments, however, could benefit from further improvements. An option for realizing some of these improvements involves introduction of discrete fibers into concrete. When compared with today's micro-scale (steel, polypropylene, glass, etc.) fibers, graphite nanomaterials (carbon nanotube, nanofiber and graphite nanoplatelet) offer superior geometric, mechanical and physical characteristics. Graphite nanomaterials would realize their reinforcement potential as far as they are thoroughly dispersed within cement-based matrices, and effectively bond to cement hydrates. The research reported herein developed non-covalent and covalent surface modification techniques to improve the dispersion and interfacial interactions of graphite nanomaterials in cement-based matrices with a dense and well graded micro-structure. The most successful approach involved polymer wrapping of nanomaterials for increasing the density of hydrophilic groups on the nanomaterial surface without causing any damage to the their structure. The nanomaterials were characterized using various spectrometry techniques, and SEM (Scanning Electron Microscopy). The graphite nanomaterials were dispersed via selected sonication procedures in the mixing water of the cement-based matrix; conventional mixing and sample preparation techniques were then employed to prepare the cement-based nanocomposite samples, which were subjected to steam curing. Comprehensive engineering and durability characteristics of cement-based nanocomposites were determined and their chemical composition, microstructure and failure mechanisms were also assessed through various spectrometry, thermogravimetry, electron microscopy and elemental analyses. Both functionalized and non-functionalized nanomaterials as well as different

  6. 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.

  7. AMS-C14 analysis of graphite obtained with an Automated Graphitization Equipment (AGE III) from aerosol collected on quartz filters

    Energy Technology Data Exchange (ETDEWEB)

    Solís, C.; Chávez, E.; Ortiz, M.E.; Andrade, E. [Instituto de Física, Universidad Nacional Autónoma de México, 04510 México D.F. (Mexico); Ortíz, E. [Universidad Autónoma Metropolitana, Unidad Azcapotzalco, México D.F. (Mexico); Szidat, S. [Department of Chemistry and Biochemistry, University of Bern, Freiestrasse 3, CH-3012 Bern (Switzerland); Paul Scherrer Institut (PSI), CH-5232 Villigen (Switzerland); Wacker, L. [Laboratory of Ion Physics, ETH, Honggerberg, Zurich (Switzerland)

    2015-10-15

    AMS-{sup 14}C applications often require the analysis of small samples. Such is the case of atmospheric aerosols where frequently only a small amount of sample is available. The ion beam physics group at the ETH, Zurich, has designed an Automated Graphitization Equipment (AGE III) for routine graphite production for AMS analysis from organic samples of approximately 1 mg. In this study, we explore the potential use of the AGE III for graphitization of particulate carbon collected in quartz filters. In order to test the methodology, samples of reference materials and blanks with different sizes were prepared in the AGE III and the graphite was analyzed in a MICADAS AMS (ETH) system. The graphite samples prepared in the AGE III showed recovery yields higher than 80% and reproducible {sup 14}C values for masses ranging from 50 to 300 μg. Also, reproducible radiocarbon values were obtained for aerosol filters of small sizes that had been graphitized in the AGE III. As a study case, the tested methodology was applied to PM{sub 10} samples collected in two urban cities in Mexico in order to compare the source apportionment of biomass and fossil fuel combustion. The obtained {sup 14}C data showed that carbonaceous aerosols from Mexico City have much lower biogenic signature than the smaller city of Cuernavaca.

  8. Use of Different Furnaces to Study Repeatability and Reproducibility of Three Pd-C Cells

    Science.gov (United States)

    Battuello, M.; Florio, M.; Girard, F.

    2010-09-01

    Three different Pd-C eutectic fixed-point cells were prepared and investigated at INRIM. Several tens of phase transition runs were carried out and recorded with both a Si-based radiation thermometer at 950 nm and a precision InGaAs-based thermometer at 1.6 μm. Two of the cells were of the same design with an inner volume of 12 cm3. The third one was smaller with a useful inner volume of 3.6 cm3. The three cells were filled with palladium powder 4N5 or 4N8 pure and graphite powder 6N pure. The repeatability and stability of the inflection point were investigated over a period of 1 year. The noticeably different external dimensions of the two cells, namely, 110 mm and 40 mm in length, allowed the influence of the longitudinal temperature distribution to be investigated. For this purpose, two different furnaces, a single-zone with SiC heaters and a three-zone with MoSi2 heaters, were used. Different operative conditions, namely, temperature steps, melting rate, longitudinal temperature distributions, and position of cells within the furnace, were tested to investigate the reproducibility of the cells. Effects on the duration and shape of the plateaux were also studied. This article gives details of the measurement setup and analyses of the melting plateaux obtained with the different conditions.

  9. Friction anisotropy in boronated graphite

    International Nuclear Information System (INIS)

    Kumar, N.; Radhika, R.; Kozakov, A.T.; Pandian, R.; Chakravarty, S.; Ravindran, T.R.; Dash, S.; Tyagi, A.K.

    2015-01-01

    Graphical abstract: - Highlights: • Friction anisotropy in boronated graphite is observed in macroscopic sliding condition. • Low friction coefficient is observed in basal plane and becomes high in prismatic direction. • 3D phase of boronated graphite transformed into 2D structure after friction test. • Chemical activity is high in prismatic plane forming strong bonds between the sliding interfaces. - Abstract: Anisotropic friction behavior in macroscopic scale was observed in boronated graphite. Depending upon sliding speed and normal loads, this value was found to be in the range 0.1–0.35 in the direction of basal plane and becomes high 0.2–0.8 in prismatic face. Grazing-incidence X-ray diffraction analysis shows prominent reflection of (0 0 2) plane at basal and prismatic directions of boronated graphite. However, in both the wear tracks (1 1 0) plane become prominent and this transformation is induced by frictional energy. The structural transformation in wear tracks is supported by micro-Raman analysis which revealed that 3D phase of boronated graphite converted into a disordered 2D lattice structure. Thus, the structural aspect of disorder is similar in both the wear tracks and graphite transfer layers. Therefore, the crystallographic aspect is not adequate to explain anisotropic friction behavior. Results of X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy shows weak signature of oxygen complexes and functional groups in wear track of basal plane while these species dominate in prismatic direction. Abundance of these functional groups in prismatic plane indicates availability of chemically active sites tends to forming strong bonds between the sliding interfaces which eventually increases friction coefficient

  10. Friction anisotropy in boronated graphite

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, N., E-mail: niranjan@igcar.gov.in [Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam (India); Radhika, R. [Crystal Growth Centre, Anna University, Chennai (India); Kozakov, A.T. [Research Institute of Physics, Southern Federal University, Rostov-on-Don (Russian Federation); Pandian, R. [Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam (India); Chakravarty, S. [UGC-DAE CSR, Kalpakkam (India); Ravindran, T.R.; Dash, S.; Tyagi, A.K. [Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam (India)

    2015-01-01

    Graphical abstract: - Highlights: • Friction anisotropy in boronated graphite is observed in macroscopic sliding condition. • Low friction coefficient is observed in basal plane and becomes high in prismatic direction. • 3D phase of boronated graphite transformed into 2D structure after friction test. • Chemical activity is high in prismatic plane forming strong bonds between the sliding interfaces. - Abstract: Anisotropic friction behavior in macroscopic scale was observed in boronated graphite. Depending upon sliding speed and normal loads, this value was found to be in the range 0.1–0.35 in the direction of basal plane and becomes high 0.2–0.8 in prismatic face. Grazing-incidence X-ray diffraction analysis shows prominent reflection of (0 0 2) plane at basal and prismatic directions of boronated graphite. However, in both the wear tracks (1 1 0) plane become prominent and this transformation is induced by frictional energy. The structural transformation in wear tracks is supported by micro-Raman analysis which revealed that 3D phase of boronated graphite converted into a disordered 2D lattice structure. Thus, the structural aspect of disorder is similar in both the wear tracks and graphite transfer layers. Therefore, the crystallographic aspect is not adequate to explain anisotropic friction behavior. Results of X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy shows weak signature of oxygen complexes and functional groups in wear track of basal plane while these species dominate in prismatic direction. Abundance of these functional groups in prismatic plane indicates availability of chemically active sites tends to forming strong bonds between the sliding interfaces which eventually increases friction coefficient.

  11. Addition of electric arc furnace dust in hot metal changing the form of addition

    International Nuclear Information System (INIS)

    Marques Sobrinho, Vicente de Paulo Ferreira; Oliveira, Jose Roberto de; Vieira, Estefano Aparecido; Telles, Victor Bridi; Grillo, Felipe Fardin; Tenorio, Jorge Alberto Soares; Espinosa, Denise Crocce Romano

    2014-01-01

    This research aims to study the incorporation of the mass of electric arc furnace dust (EAFD), by addition in hot metal (1.78% Si) at a temperature of 1,400 degrees Celsius. The EAFD is from a steel plant producing long steel. The addition of the EAFD was as received, in the form of briquettes without agitation of the hot metal and in the form of briquettes with agitation of the hot metal. Previously, the EAFD was characterized using the following techniques: chemical analysis, size analysis, X-ray diffraction, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) microanalysis. The achievement of fusion experiments in laboratory scale, took place in a vertical tubular furnace with temperature control. The fusion experiments to assess the incorporation of EAFD mass used graphite crucibles. After cooling, the hot metal and the slag, remaining in the crucible, were weighed to do a mass balance. A flow of inert gas (argon) was maintained inside the furnace during the experiments. Results show that the experiment with addition of EAFD as received presents the best result of incorporating the mass of the final hot metal (1.73%) combined with the lowest percentage of volatilized mass of EAFD (46.52%). The experiment addition of EAFD in the form of briquette with agitation of hot metal presents the lowest percentage of slag mass (4.58%). The zinc content of volatilized EAFD (64.30%) is higher than the zinc content of the imported ore concentrate (52%) and zinc content of the national ore concentrate (12% to 39%). The presence of lead and cadmium in the slag characterizing it as a hazardous solid waste. (author)

  12. Use of graphite layer open tubular (GLOT) in environmental analysis

    International Nuclear Information System (INIS)

    Bruner, F.; Lattanzi, L.; Borghesi, P.

    1996-01-01

    Recently it has been developed a series of new capillary columns characterised by the use of graphitized carbon black modified from different amount of liquid phase. The characteristics of these columns, called graphite layer open tubular (GLOT), are described together with their application to the environmental analysis. A specific application of GLOT columns is for the direct analysis of aqueous solutions avoiding solvent extraction procedure. A comparison between a GLOT column and a traditional capillary column, estimating their behaviour after repeated direct injections of aqueous solution sample is written. Some applications regarding the analysis of the atmosphere pollutants, as aliphatic and aromatic hydrocarbons, and their compounds are written too

  13. Pencil graphite leads as simple amperometric sensors for microchip electrophoresis.

    Science.gov (United States)

    Natiele Tiago da Silva, Eiva; Marques Petroni, Jacqueline; Gabriel Lucca, Bruno; Souza Ferreira, Valdir

    2017-11-01

    In this work we demonstrate, for the first time, the use of inexpensive commercial pencil graphite leads as simple amperometric sensors for microchip electrophoresis. A PDMS support containing one channel was fabricated through soft lithography and sanded pencil graphite leads were inserted into this channel to be used as working electrodes. The electrochemical and morphological characterization of the sensor was carried out. The graphite electrode was coupled to PDMS microchips in end-channel configuration and electrophoretic experiments were performed using nitrite and ascorbate as probe analytes. The analytes were successfully separated and detected in well-defined peaks with satisfactory resolution using the microfluidic platform proposed. The repeatability of the pencil graphite electrode was satisfactory (RSD values of 1.6% for nitrite and 12.3% for ascorbate, regarding the peak currents) and its lifetime was estimated to be ca. 700 electrophoretic runs over a cost of ca. $ 0.05 per electrode. The limits of detection achieved with this system were 2.8 μM for nitrite and 5.7 μM for ascorbate. For proof of principle, the pencil graphite electrode was employed for the real analysis of well water samples and nitrite was successfully quantified at levels below its maximum contaminant level established in Brazil and US. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. From Graphite to Graphene via Scanning Tunneling Microscopy

    Science.gov (United States)

    Qi, Dejun

    The primary objective of this dissertation is to study both graphene on graphite and pristine freestanding grapheme using scanning tunneling microscopy (STM) and density functional theory (DFT) simulation technique. In the experiment part, good quality tungsten metalic tips for experiment were fabricated using our newly developed tip making setup. Then a series of measurements using a technique called electrostatic-manipulation scanning tunneling microscopy (EM-STM) of our own development were performed on a highly oriented pyrolytic graphite (HOPG) surface. The electrostatic interaction between the STM tip and the sample can be tuned to produce both reversible and irreversible large-scale movement of the graphite surface. Under this influence, atomic-resolution STM images reveal that a continuous electronic transition between two distinct patterns can be systematically controlled. DFT calculations reveal that this transition can be related to vertical displacements of the top layer of graphite relative to the bulk. Evidence for horizontal shifts in the top layer of graphite is also presented. Excellent agreement is found between experimental STM images and those simulated using DFT. In addition, the EM-STM technique was also used to controllably and reversibly pull freestanding graphene membranes up to 35 nm from their equilibrium height. Atomic-scale corrugation amplitudes 20 times larger than the STM electronic corrugation for graphene on a substrate were observed. The freestanding graphene membrane responds to a local attractive force created at the STM tip as a highly conductive yet flexible grounding plane with an elastic restoring force.

  15. Sealed rotary hearth furnace with central bearing support

    Science.gov (United States)

    Docherty, James P.; Johnson, Beverly E.; Beri, Joseph

    1989-01-01

    The furnace has a hearth which rotates inside a stationary closed chamber and is supported therein on vertical cylindrical conduit which extends through the furnace floor and is supported by a single center bearing. The charge is deposited through the furnace roof on the rim of the hearth as it rotates and is moved toward the center of the hearth by rabbles. Externally generated hot gases are introduced into the furnace chamber below the hearth and rise through perforations in the hearth and up through the charge. Exhaust gases are withdrawn through the furnace roof. Treated charge drops from a center outlet on the hearth into the vertical cylindrical conduit which extends downwardly through the furnace floor to which it is also sealed.

  16. Application of Carbon Composite Bricks for Blast Furnace Hearth

    Science.gov (United States)

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

    Traditional refractory materials for blast furnace hearth lining are mainly composed of carbon bricks and the ceramic cup. However, these materials can't meet the demands for long service life design of blast furnaces. In this paper, a new refractory called carbon composite brick (CCB) was introduced, which combined the advantages of carbon bricks and the ceramic cup. In this case, the resistance of the CCB against corrosion was equal to the ceramic cup and the thermal conductivity of the CCB was equal to carbon bricks. From the results of more than 20 blast furnaces, the CCB could be well used in small blast furnaces and large blast furnaces. In the bad condition of low grade burden and high smelting intensity, the CCB gave full play to the role of cooling system, and effectively resisted the erosion of hot metal to improve the service life of blast furnaces.

  17. Nanodiamond graphitization: a magnetic resonance study

    International Nuclear Information System (INIS)

    Panich, A M; Shames, A I; Sergeev, N A; Olszewski, M; McDonough, J K; Mochalin, V N; Gogotsi, Y

    2013-01-01

    We report on the first nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR) study of the high-temperature nanodiamond-to-onion transformation. 1 H, 13 C NMR and EPR spectra of the initial nanodiamond samples and those annealed at 600, 700, 800 and 1800 ° C were measured. For the samples annealed at 600 to 800 ° C, our NMR data reveal the early stages of the surface modification, as well as a progressive increase in sp 2 carbon content with increased annealing temperature. Such quantitative experimental data were recorded for the first time. These findings correlate with EPR data on the sensitivity of the dangling bond EPR line width to air content, progressing with rising annealing temperature, that evidences consequent graphitization of the external layers of the diamond core. The sample annealed at 1800 ° C shows complete conversion of nanodiamond particles into carbon onions. (paper)

  18. Fabrication of Graphene by Cleaving Graphite Chemically

    Institute of Scientific and Technical Information of China (English)

    ZHAO Shu-hua; ZHAO Xiao-ting; FAN Hou-gang; YANG Li-li; ZHANG Yong-jun; YANG Jing-hai

    2011-01-01

    Graphite was chemically cleaved to graphene by Billups Reaction,and the morphologies and microstructures of graphene were characterized by SEM,Raman and AFM.The results show that the graphite was first functionalized by l-iodododecane,which led to the cleavage of the graphene layer in the graphite.The second decoration cleaved the graphite further and graphene was obtained.The heights of the graphene layer were larger than 1 nm due to the organic decoration.

  19. 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.

  20. Assessment of selected furnace technologies for RWMC waste

    International Nuclear Information System (INIS)

    Batdorf, J.; Gillins, R.; Anderson, G.L.

    1992-03-01

    This report provides a description and initial evaluation of five selected thermal treatment (furnace) technologies, in support of earlier thermal technologies scoping work for application to the Idaho National Engineering Laboratory Radioactive Waste Management Complex (RWMC) buried wastes. The cyclone furnace, molten salt processor, microwave melter, ausmelt (fuel fired lance) furnace, and molten metal processor technologies are evaluated. A system description and brief development history are provided. The state of development of each technology is assessed, relative to treatment of RWMC buried waste

  1. Baking and helium glow discharge cleaning of SST-1 tokamak with graphite plasma facing components

    International Nuclear Information System (INIS)

    Semwal, Pratibha; Khan, Ziauddin; Raval, Dilip

    2015-01-01

    Graphite plasma facing components (PFCs) were installed inside SST-1 vacuum vessel. Prior to installation, all the graphite tiles were baked at 1000 °C in a vacuum furnace operated below 1.0 X 10 -5 mbar. However due to the porous structure of graphite, they absorb a significant amount of water vapour from air during the installation process. Rapid desorption of water vapour requires high temperature bake-out of the PFCs at ≥ 250 °C. In SST-1 the PFCs were baked at 250 °C using hot nitrogen gas facility to remove the absorbed water vapour. Also device with large graphite surface area has the disadvantage that a large quantity of hydrogen gets trapped inside it during plasma discharges which makes density control difficult. Helium (He) glow discharge cleaning (GDC) effectively removes this stored hydrogen as well as other impurities like oxygen and hydrocarbon within few nanometers from the surface by particle induced desorption. Before plasma operation in SST-1 tokamak, both baking of PFCs and He-GDC were carried out so that these impurities were removed effectively. The mean desorption yield of hydrogen was found to be 0.48. In this paper, the results of effect of baking and He-GDC experiments of SST-1 will be presented in detail. (author)

  2. Baking and helium glow discharge cleaning of SST-1 Tokamak with graphite plasma facing components

    International Nuclear Information System (INIS)

    Semwal, P; Khan, Z; Raval, D C; Dhanani, K R; George, S; Paravastu, Y; Prakash, A; Thankey, P; Ramesh, G; Khan, M S; Saikia, P; Pradhan, S

    2017-01-01

    Graphite plasma facing components (PFCs) were installed inside the SST-1 vacuum vessel. Prior to installation, all the graphite tiles were baked at 1000 °C in a vacuum furnace operated below 1.0 × 10 -5 mbar. However due to the porous structure of graphite, they absorb a significant amount of water vapour from air during the installation process. Rapid desorption of this water vapour requires high temperature bake-out of the PFCs at ≥ 250 °C. In SST-1 the PFCs were baked at 250 °C using hot nitrogen gas facility to remove the absorbed water vapour. Also device with large graphite surface area has the disadvantage that a large quantity of hydrogen gets trapped inside it during plasma discharges which makes density control difficult. Helium glow discharge cleaning (He-GDC) effectively removes this stored hydrogen as well as other impurities like oxygen and hydrocarbon within few nano-meters from the surface by particle induced desorption. Before plasma operation in SST-1 tokamak, both baking of PFCs and He-GDC were carried out so that these impurities were removed effectively. The mean desorption yield of hydrogen was found to be 0.24. In this paper the results of baking and He-GDC experiments of SST-1 will be presented in detail. (paper)

  3. Baking and helium glow discharge cleaning of SST-1 Tokamak with graphite plasma facing components

    Science.gov (United States)

    Semwal, P.; Khan, Z.; Raval, D. C.; Dhanani, K. R.; George, S.; Paravastu, Y.; Prakash, A.; Thankey, P.; Ramesh, G.; Khan, M. S.; Saikia, P.; Pradhan, S.

    2017-04-01

    Graphite plasma facing components (PFCs) were installed inside the SST-1 vacuum vessel. Prior to installation, all the graphite tiles were baked at 1000 °C in a vacuum furnace operated below 1.0 × 10-5 mbar. However due to the porous structure of graphite, they absorb a significant amount of water vapour from air during the installation process. Rapid desorption of this water vapour requires high temperature bake-out of the PFCs at ≥ 250 °C. In SST-1 the PFCs were baked at 250 °C using hot nitrogen gas facility to remove the absorbed water vapour. Also device with large graphite surface area has the disadvantage that a large quantity of hydrogen gets trapped inside it during plasma discharges which makes density control difficult. Helium glow discharge cleaning (He-GDC) effectively removes this stored hydrogen as well as other impurities like oxygen and hydrocarbon within few nano-meters from the surface by particle induced desorption. Before plasma operation in SST-1 tokamak, both baking of PFCs and He-GDC were carried out so that these impurities were removed effectively. The mean desorption yield of hydrogen was found to be 0.24. In this paper the results of baking and He-GDC experiments of SST-1 will be presented in detail.

  4. 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.

  5. 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

  6. 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.

  7. NMR studies on graphite-methanol system

    International Nuclear Information System (INIS)

    El-Akkad, T.M.

    1977-01-01

    The nuclear magnetic relaxation times for protons of methanol on graphite have been studied. The perpendicular and the transversal magnetization as a function of temperature were measured. The results show that the presence of graphite slowed down the methanol movement compared with that in the pure alcohol, and that the methanol molecules are attached to the graphite surface via methyl groups. (author)

  8. Characterization of the permeability of the blast furnace lower part

    International Nuclear Information System (INIS)

    Negro, P.; Petit, C.; Urvoy, A.; Sert, D.; Pierret, H.

    2001-01-01

    In the context of high coal injection and high productivity operation, the coke behaviour inside the blast furnace hearth is the main parameter to control. Different and complementary investigations as radioactive and helium tracer injections, liquids and coke samplings, have been carried out at Sollac Fos BF1 using the tuyere probe to determine the hearth permeability and its evolutions as a function of the main control parameters, and to understand the hearth activity. The results of all these experiments give a very consistent picture of a heterogenous hearth with three concentric areas of various permeabilities to gas and liquids. A two concentric zones model has been built, which is in good agreement with the experimental results. It enables to evaluate the impact of the central zone on the liquids flow at the periphery. (author)

  9. Characterization of electric arc furnace dust aiming reuse

    International Nuclear Information System (INIS)

    Grillo, F.F.; Oliveira, E.B.G.; Oliveira, J.R. de; Telles, V.B.; Tenorio, J.A.S.

    2010-01-01

    This work aims to study the characterize of steelmaking dust, from the primary refining of steel in Electric Arc Furnace, in order to verify feasibility of reuse through the addition of hot metal in the form of briquette. The techniques used to characterize the dust was chemical analyses, size separation tests, X-ray diffraction analyses (XRD), Scanning Electron Microscopy (SEM). After characterization, was the calculation of reductant considering the complete reduction of iron oxides and then to briquetting. The waste sample is composed essentially of spherical particles and has a very small particle size (85% below 10 μm). The XRD has presented compounds such as ZnFe 2 O 4 , Fe 3 O 4 , ZnO e SiO 2 . This work showed that its possible recovery approximately 92% of metal iron from dust generated during steelmaking.This (author)

  10. Predictive control of thermal state of blast furnace

    Science.gov (United States)

    Barbasova, T. A.; Filimonova, A. A.

    2018-05-01

    The work describes the structure of the model for predictive control of the thermal state of a blast furnace. The proposed model contains the following input parameters: coke rate; theoretical combustion temperature, comprising: natural gas consumption, blasting temperature, humidity, oxygen, blast furnace cooling water; blast furnace gas utilization rate. The output parameter is the cast iron temperature. The results for determining the cast iron temperature were obtained following the identification using the Hammerstein-Wiener model. The result of solving the cast iron temperature stabilization problem was provided for the calculated values of process parameters of the target area of the respective blast furnace operation mode.

  11. Comprehensive Numerical Modeling of the Blast Furnace Ironmaking Process

    Science.gov (United States)

    Zhou, Chenn; Tang, Guangwu; Wang, Jichao; Fu, Dong; Okosun, Tyamo; Silaen, Armin; Wu, Bin

    2016-05-01

    Blast furnaces are counter-current chemical reactors, widely utilized in the ironmaking industry. Hot reduction gases injected from lower regions of the furnace ascend, reacting with the descending burden. Through this reaction process, iron ore is reduced into liquid iron that is tapped from the furnace hearth. Due to the extremely harsh environment inside the blast furnace, it is difficult to measure or observe internal phenomena during operation. Through the collaboration between steel companies and the Center for Innovation through Visualization and Simulation, multiple computational fluid dynamics (CFD) models have been developed to simulate the complex multiphase reacting flow in the three regions of the furnace, the shaft, the raceway, and the hearth. The models have been used effectively to troubleshoot and optimize blast furnace operations. In addition, the CFD models have been integrated with virtual reality. An interactive virtual blast furnace has been developed for training purpose. This paper summarizes the developments and applications of blast furnace CFD models and the virtual blast furnace.

  12. Nitrogen oxide emissions from a kraft recovery furnace

    International Nuclear Information System (INIS)

    Prouty, A.L.; Stuart, R.C.; Caron, A.L.

    1993-01-01

    Nitrogen Oxide (NOx) emissions from a rebuilt kraft recovery furnace slightly exceeded the specified limit of 1.1 lb/ton (0.55 kg/metric ton) of black-liquor solids. Mill trials were undertaken to determine whether NOx emissions could be minimized by modifying furnace operation. NOx emissions increased when secondary air was shifted to tertiary ports. NOx emissions fell when the amounts of primary and total air were decreased, but this increased emissions of other pollutants. After demonstrating that best operation of the furnace could not meet the permit with an emissions limit that matched the furnace's performance at best operation

  13. A review of temperature measurement in the steel reheat furnace

    International Nuclear Information System (INIS)

    Martocci, A.P.; Mihalow, F.A.

    1985-01-01

    The incentive for conducting research and development on reheat furnaces is substantial; the domestic steel industry spent approximately one billion dollars on fuel in reheat furnaces in 1981. Bethlehem Steel Corp. spent /145 million of that total, and neither figure includes fuel consumed in soaking pits or annealing furnaces. If the authors set a goal to save 10% of these annual fuel costs, that translates into /100 million for the domestic steel industry and /14.5 million for Bethlehem Steel. These large sums of money are significant incentives. The purpose of this paper is to review the historical heating practices and equipment at steel reheat furnaces along with current practices and instrumentation

  14. Development of Nanoscale Graphitic Devices and The Transport Characterization

    International Nuclear Information System (INIS)

    Gunasekaran, Venugopal

    2011-02-01

    This dissertation describes the development of graphitic based nanoscale devices with its fabrication and transport characterization results. It covers graphite nano-scale stacked-junctions fabricated using focused ion beam (FIB) 3-D etching technique, a single layer graphite layer (graphene) preparation and its electrical transport characterization results and the synthesis and investigation of electrical transport behavior of graphene oxide based thin film devices. The first chapter describes the basic information about the carbon family in detail in which the electronic properties and structure of graphite, graphene and graphene oxide are discussed. In addition, the necessity of developing nanoscale graphitic devices is given. The second chapter explains the experimental techniques used in this research for fabricating nanoscale devices which includes focused ion beam 3-D fabrication procedures, mechanical exfoliation technique and photolithographic methods. In third chapter, we have reported the results on temperature dependence of graphite planar-type structures fabricated along ab-plane. In the fourth and fifth chapters, the fabrication and electrical transport characteristics of large in-plane area graphite planar-type structures (fabricated along ab-plane and c-axis) were discussed and their transport anisotropy properties were investigated briefly. In the sixth chapter, we focused the fabrication of the submicron sized graphite stacked junctions and their electrical transport characterization studies. In which, FIB was used to fabricated the submicron junctions with various in-plane area (with same stack height) are and their transport characteristics were compared. The seventh chapter reports investigation of electrical transport results of nanoscale graphite stacked-junctions in which the temperature dependent transport (R-T) studies, current-voltage measurements for the various in-plane areas and for various stack height samples were analyzed. The

  15. Continuous denitration device using a microwave furnace

    International Nuclear Information System (INIS)

    Sato, Hajime

    1982-04-01

    A continuous denitration device is described that enables to obtain dried U or Pu dioxide or a mixture of these from a solution of uranyl or plutonium nitrate or a mixed solution of these by irradiation with microwaves. This device allows uranyl or plutonium nitrate to crystallize and the resulting crystals to be separated from the solution. A belt conveyer carries the crystals to a microwave heating furnace for denitration. Approximately 2.4 kg dried cake of U dioxide per hour is obtained [fr

  16. Oil injection into the blast furnace

    Energy Technology Data Exchange (ETDEWEB)

    Dongsheng Liao; Mannila, P.; Haerkki, J.

    1997-12-31

    Fuel injection techniques have been extensively used in the commercial blast furnaces, a number of publications concerning the fuels injection have been reported. This present report only summarizes the study achievements of oil injection due to the research need the of authors, it includes the following parts: First, the background and the reasons reducing coke rate of oil injection are analyzed. Reducing coke rate and decreasing the ironmaking costs are the main deriving forces, the contents of C, H and ash are direct reasons reducing coke rate. It was also found that oil injection had great effects on the state of blast furnace, it made operation stable, center gas flow develop fully, pressure drop increase, descent speed of burden materials decrease and generation of thermal stagnation phenomena, the quality of iron was improved. Based on these effects, as an ideal mean, oil injection was often used to adjust the state of blast furnace. Secondly, combustion behavior of oil in the raceway and tuyere are discussed. The distribution of gas content was greatly changed, the location of CO, H{sub 2} generation was near the tuyere; the temperature peak shifts from near the raceway boundary to the tuyere. Oxygen concentration and blast velocity were two important factors, it was found that increasing excess oxygen ratio 0.9 to 1.3, the combustion time of oil decreases 0.5 msec, an increase of the blast velocity results in increasing the flame length. In addition, the nozzle position and oil rate had large effects on the combustion of oil. Based on these results, the limit of oil injection is also discussed, soot formation is the main reason limiting to further increase oil injection rate, it was viewed that there were three types of soot which were generated under blast furnace operating conditions. The reason generating soot is the incomplete conversion of the fuel. Finally, three methods improving combustion of oil in the raceway are given: Improvement of oil

  17. 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.

  18. 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 siliconcarbide 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 considers 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.

  19. Superconductivity in graphite intercalation compounds

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Robert P. [Cavendish Laboratory, University of Cambridge, Madingley Road, Cambridge CB3 0HE (United Kingdom); Weller, Thomas E.; Howard, Christopher A. [Department of Physics & Astronomy, University College of London, Gower Street, London WCIE 6BT (United Kingdom); Dean, Mark P.M. [Department of Condensed Matter Physics and Materials Science, Brookhaven National Laboratory, Upton, NY 11973 (United States); Rahnejat, Kaveh C. [Department of Physics & Astronomy, University College of London, Gower Street, London WCIE 6BT (United Kingdom); Saxena, Siddharth S. [Cavendish Laboratory, University of Cambridge, Madingley Road, Cambridge CB3 0HE (United Kingdom); Ellerby, Mark, E-mail: mark.ellerby@ucl.ac.uk [Department of Physics & Astronomy, University College of London, Gower Street, London WCIE 6BT (United Kingdom)

    2015-07-15

    Highlights: • Historical background of graphite intercalates. • Superconductivity in graphite intercalates and its place in the field of superconductivity. • Recent developments. • Relevant modeling of superconductivity in graphite intercalates. • Interpretations that pertain and questions that remain. - Abstract: The field of superconductivity in the class of materials known as graphite intercalation compounds has a history dating back to the 1960s (Dresselhaus and Dresselhaus, 1981; Enoki et al., 2003). This paper recontextualizes the field in light of the discovery of superconductivity in CaC{sub 6} and YbC{sub 6} in 2005. In what follows, we outline the crystal structure and electronic structure of these and related compounds. We go on to experiments addressing the superconducting energy gap, lattice dynamics, pressure dependence, and how these relate to theoretical studies. The bulk of the evidence strongly supports a BCS superconducting state. However, important questions remain regarding which electronic states and phonon modes are most important for superconductivity, and whether current theoretical techniques can fully describe the dependence of the superconducting transition temperature on pressure and chemical composition.

  20. Superconductivity in graphite intercalation compounds

    International Nuclear Information System (INIS)

    Smith, Robert P.; Weller, Thomas E.; Howard, Christopher A.; Dean, Mark P.M.; Rahnejat, Kaveh C.; Saxena, Siddharth S.; Ellerby, Mark

    2015-01-01

    Highlights: • Historical background of graphite intercalates. • Superconductivity in graphite intercalates and its place in the field of superconductivity. • Recent developments. • Relevant modeling of superconductivity in graphite intercalates. • Interpretations that pertain and questions that remain. - Abstract: The field of superconductivity in the class of materials known as graphite intercalation compounds has a history dating back to the 1960s (Dresselhaus and Dresselhaus, 1981; Enoki et al., 2003). This paper recontextualizes the field in light of the discovery of superconductivity in CaC 6 and YbC 6 in 2005. In what follows, we outline the crystal structure and electronic structure of these and related compounds. We go on to experiments addressing the superconducting energy gap, lattice dynamics, pressure dependence, and how these relate to theoretical studies. The bulk of the evidence strongly supports a BCS superconducting state. However, important questions remain regarding which electronic states and phonon modes are most important for superconductivity, and whether current theoretical techniques can fully describe the dependence of the superconducting transition temperature on pressure and chemical composition

  1. 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.

  2. 'In situ' expanded graphite extinguishant

    International Nuclear Information System (INIS)

    Cao Qixin; Shou Yuemei; He Bangrong

    1987-01-01

    This report is concerning the development of the extinguishant for sodium fire and the investigation of its extinguishing property. The experiment result shows that 'in situ' expanded graphite developed by the authors is a kind of extinguishant which extinguishes sodium fire quickly and effectively and has no environment pollution during use and the amount of usage is little

  3. 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

  4. Feasibility of monitoring the strength of HTGR core support graphite. Part II

    International Nuclear Information System (INIS)

    Morgan, W.C.; Becker, F.L.

    1979-08-01

    The results reported establish the technical feasibility of a method for monitoring the strength of HTGR core support structures in situ. Correlations have been established between the velocity of an ultrasonic pulse and the compressive strength of four different grades of graphite. For some grades of graphite, one or more of the correlations are practically independent of oxidation profile in samples having cylindrical geometry (as in the core support posts). For other grades of graphite, and for other sample geometries, the oxidation-depth profile must be known in order to reliably predict the effect of oxidation on compressive strength

  5. A new graphite preparation line for AMS 14C dating in the Zagreb Radiocarbon Laboratory

    Science.gov (United States)

    Krajcar Bronić, I.; Horvatinčić, N.; Sironić, A.; Obelić, B.; Barešić, J.; Felja, I.

    2010-04-01

    The new line for preparation of graphite samples for 14C dating by AMS has been constructed in the Zagreb Radiocarbon Laboratory. The performance of the rig and sample preparation procedure has been validated by preparing graphites from various reference materials of known 14C activity. The yield of the graphitization was good and the measured fraction of modern carbon ( Fm) values have not significantly deviated from the expected ones. Detailed analysis of measured Fm values indicates a slight bias to more positive values and should be carefully investigated.

  6. Determining misorientation of graphite grains from the angular dependence of X-ray emission spectra

    International Nuclear Information System (INIS)

    Belavin, V. V.; Okotrub, A. V.; Bulusheva, L. G.; Kotosonov, A. S.; Vyalykh, D. V.; Molodtsov, S. L.

    2006-01-01

    Angular-resolved X-ray absorption spectra were measured for pyrolytic graphite samples of various quality. A new approach to determining the misorientation of graphite grains in polycrystalline samples is proposed, which is based on calculations of the angular dependence of the relative intensity of a peak corresponding to the π* state for a normal distribution of grains. The experimental values are used to construct theoretical angular dependences using partial densities of the π* and σ* states determined from the nonempirical calculations for graphite

  7. Graphite suspension in carbon dioxide

    International Nuclear Information System (INIS)

    Roche, R.

    1965-01-01

    Since 1963 the Atomic Division of SNECMA has been conducting, under a contract with the CEA, an experimental work with a two-component fluid comprised of carbon dioxide and small graphite particles. The primary purpose was the determination of basic engineering information pertaining to the stability and the flowability of the suspension. The final form of the experimental loop consists mainly of the following items: a light-phase compressor, a heavy-phase pump, an electrical-resistance type heater section, a cooling heat exchanger, a hairpin loop, a transparent test section and a separator. During the course of the testing, it was observed that the fluid could be circulated quite easily in a broad range of variation of the suspension density and velocity - density from 30 to 170 kg/m 3 and velocity from 2 to 24 m/s. The system could be restarted and circulation maintained without any difficulty, even with the heavy-phase pump alone. The graphite did not have a tendency to pack or agglomerate during operation. No graphite deposition was observed on the wall of the tubing. A long period run (250 hours) has shown the evolution of the particle dimensions. Starting with graphite of surface area around 20 m 2 /g (graphite particles about 1 μ), the powder surface area reaches an asymptotic value of 300 m 2 /g (all the particles less than 0.3 μ). Moisture effect on flow stability, flow distribution between two parallel channels, pressure drop in straight tubes, recompression ratio in diffusers were also investigated. (author) [fr

  8. 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

    2016-03-14

    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.

  9. Aluminum-graphite composite produced by mechanical milling and hot extrusion

    International Nuclear Information System (INIS)

    Flores-Zamora, M.I.; Estrada-Guel, I.; Gonzalez-Hernandez, J.; Miki-Yoshida, M.; Martinez-Sanchez, R.

    2007-01-01

    Aluminum-graphite composites were produced by mechanical milling followed by hot extrusion. Graphite content was varied between 0 and 1 wt.%. Al-graphite mixtures were initially mixed in a shaker mill without ball, followed by mechanical milling in a High-energy simoloyer mill for 2 h under argon atmosphere. Milled powders were subsequently pressed at ∼950 MPa for 2 min, and next sintered under vacuum for 3 h at 823 K. Finally, sintered products were held for 0.5 h at 823 K and hot extruded using indirect extrusion. Tension and compression tests were carried out to determine the yield stress and maximum stress of the materials. We found that the mechanical resistance increased as the graphite content increased. Microstructural characterization was done by transmission electron microscopy. Al-O-C nanofibers and graphite nanoparticles were observed in extruded samples by transmission electron microscopy. These nanoparticles and nanofibers seemed to be responsible of the reinforcement phenomenon

  10. A reliability based stress-life evaluation of aluminium-graphite particulate composites

    International Nuclear Information System (INIS)

    Achutha, M.V.; Sridhara, B.K.; Abdul Budan, D.

    2008-01-01

    Fatigue tests were conducted on sand cast aluminium-graphite composite specimens on Rotating Beam Fatigue Testing Machine with three different stress levels. Aluminium-graphite (LM 25-5% graphite) composite was processed by closed mould sand casting method. Three-stress level fatigue test program was planned for carrying out fatigue experiments. Three different stress levels selected for fatigue experiments were a fraction of ultimate tensile strength. Statistical design of fatigue experiments was carried out to determine the sample size at each stress level. Experimental results are presented in the form of stress-life (S-N) curves and reliability-stress-life (R-S-N) curves, which are helpful for designers. The S-N curve of the aluminium-graphite composite was compared with its matrix alloy LM 25. Comparison revealed that the fatigue behaviour of the aluminium-graphite composite is superior to that of the matrix alloy

  11. Change of properties after oxidation of IG-11 graphite by air and CO2 gas

    International Nuclear Information System (INIS)

    Lim, Yun-Soo; Chi, Se-Hwan; Cho, Kwang-Yun

    2008-01-01

    Artificial graphite is typically manufactured by carbonization of a shaped body of a kneaded mixture using granular cokes as a filler and pitch as a binder. It undergoes a pitch impregnation process if necessary and finally applying graphitization heat treatment. The effect of thermal oxidation in air or a CO 2 atmosphere on IG-11 graphite samples is investigated in this study. The results show a localized oxidation process that progressively reveals the large coke particles with increasing level of overall weight loss in air. The surface of the graphite was peeled off and no change was found in the specific gravity after air oxidation. However, the specific gravity of graphite was continuously decreased by CO 2 oxidation. The decrease in the specific gravity by CO 2 oxidation was due to CO 2 gas that progressed from the surface to the interior. The pore shape after CO 2 oxidation differed from that under air oxidation

  12. Optimization of Sealed Tube Graphitization Method for Environmental C-14 Studies Using MICADAS

    Energy Technology Data Exchange (ETDEWEB)

    Rinyu, Laszlo, E-mail: rinyu@atomki.hu [Hertelendi Laboratory of Environmental Studies, Institute of Nuclear Research of the Hungarian Academy of Sciences (ATOMKI), H-4026 Debrecen (Hungary); Isotoptech Zrt., H-4025 Debrecen (Hungary); Molnar, Mihaly [Hertelendi Laboratory of Environmental Studies, Institute of Nuclear Research of the Hungarian Academy of Sciences (ATOMKI), H-4026 Debrecen (Hungary); Ion Beam Physics, ETH Zuerich, CH-8093 Zuerich (Switzerland); Major, Istvan [Hertelendi Laboratory of Environmental Studies, Institute of Nuclear Research of the Hungarian Academy of Sciences (ATOMKI), H-4026 Debrecen (Hungary); Nagy, Tamas; Veres, Mihaly [Isotoptech Zrt., H-4025 Debrecen (Hungary); Kimak, Adam [University of Debrecen, H-4032 Debrecen (Hungary); Wacker, Lukas; Synal, Hans-Arno [Ion Beam Physics, ETH Zuerich, CH-8093 Zuerich (Switzerland)

    2013-01-15

    The original sealed tube zinc reduction graphitization process was first developed for rapid low-precision measurements of biomedical tracer samples and later also applied for high precision measurements of not too old samples. In this study we tested the MICADAS (mini radiocarbon dating system [1]) radiocarbon measurements of targets prepared by sealed tube graphitization process. We found the optimal iron catalyst and reagents (TiH{sub 2} and Zn) amount whereby we can reach a relatively low background level, and minimized the overall {delta}{sup 13}C fractionation during the graphitization. Repeated measurements of normalization standards and real samples with known {sup 14}C activities were very well reproduced. Finally, we demonstrated the applicability of the sealed tube graphitization on real environmental samples covering a wide range of {sup 14}C concentrations.

  13. 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

  14. Reactor as furnace and reactor as lamp

    International Nuclear Information System (INIS)

    Goldanskii, V.I.

    1992-01-01

    There are presented general characteristics of the following ways of transforming of nuclear energy released in reactors into chemical : ordinary way (i.e. trough the heat, mechanical energy and electricity); chemonuclear synthesis ; use of high-temperature fuel elements (reactor as furnace); use of the mixed nγ-radiation of reactors; use of the radiation loops; radiation - photochemical synthesis (reactor as lamp). Advantage and disadvantages of all above variants are compared. The yield of the primary product of fixation of nitrogen (nitric oxide NO) in reactor with the high-temperature (above ca. 1900degC) fuel elements (reactor-furnace) can exceed W ∼ 200 kg per gram of burned uranium. For the latter variant (reactor-lamp) the yield of chemical products can reach W ∼ 60 kg. per gram of uranium. Such values of W are close to or even strongly exceed the yields of chemical products for other abovementioned variants and - what is particularly important - are not connected to the necessity of archscrupulous removal of radioactive contamination of products. (author)

  15. Energy Efficiency Model for Induction Furnace

    Science.gov (United States)

    Dey, Asit Kr

    2018-01-01

    In this paper, a system of a solar induction furnace unit was design to find out a new solution for the existing AC power consuming heating process through Supervisory control and data acquisition system. This unit can be connected directly to the DC system without any internal conversion inside the device. The performance of the new system solution is compared with the existing one in terms of power consumption and losses. This work also investigated energy save, system improvement, process control model in a foundry induction furnace heating framework corresponding to PV solar power supply. The results are analysed for long run in terms of saving energy and integrated process system. The data acquisition system base solar foundry plant is an extremely multifaceted system that can be run over an almost innumerable range of operating conditions, each characterized by specific energy consumption. Determining ideal operating conditions is a key challenge that requires the involvement of the latest automation technologies, each one contributing to allow not only the acquisition, processing, storage, retrieval and visualization of data, but also the implementation of automatic control strategies that can expand the achievement envelope in terms of melting process, safety and energy efficiency.

  16. Emission spectroscopy for coal-fired cyclone furnace diagnostics

    Energy Technology Data Exchange (ETDEWEB)

    Wehrmeyer, J.A.; Boll, D.E.; Smith, R. [Vanderbilt University, Nashville, TN (United States). Dept. of Mechanical Engineering

    2003-08-01

    Using a spectrograph and charge-coupled device (CCD) camera, ultraviolet and visible light emission spectra were obtained from a coal-burning electric utility's cyclone furnaces operating at either fuel-rich or fuel-lean conditions. The aim of this effort is to identify light emission signals that can be related to a cyclone furnace's operating condition in order to adjust its air/fuel ratio to minimize pollutant production. Emission spectra at the burner and outlet ends of cyclone furnaces were obtained. Spectra from all cyclone burners show emission lines for the trace elements Li, Na, K, and Rb, as well as the molecular species OH and CaOH. The Ca emission line is detected at the burner end of both the fuel-rich and fuellean cyclone furnaces but is not detected at the outlet ends of either furnace type. Along with the disappearance of Ca is a concomitant increase in the CaOH signal at the outlet end of both types of furnaces. The OH signal strength is in general stronger when viewing at the burner end rather than the exhaust end of both the fuel-rich and fuel-lean cyclone furnaces, probably due to high, non-equilibrium amounts of OH present inside the furnace. Only one molecular species was detected that could be used as a measure of air/fuel ratio: MgOH. It was detected at the burner end of fuel-rich cyclone furnaces but not detected in fuel-lean cyclone furnaces. More direct markers of air/fuel ratio, such as CO and 02 emission, were not detected, probably due to the generally weak nature of molecular emission relative to ambient blackbody emission present in the cyclone furnaces, even at ultraviolet wavelengths.

  17. Preparation and characterization of copper-graphite composites by electrical explosion of wire in liquid.

    Science.gov (United States)

    Bien, T N; Gul, W H; Bac, L H; Kim, J C

    2014-11-01

    Copper-graphite nanocomposites containing 5 vol.% graphite were prepared by a powder metallurgy route using an electrical wire explosion (EEW) in liquid method and spark plasma sintering (SPS) process. Graphite rods with a 0.3 mm diameter and copper wire with a 0.2 mm diameter were used as raw materials for EEWin liquid. To compare, a pure copper and copper-graphite mixture was also prepared. The fabricated graphite was in the form of a nanosheet, onto which copper particles were coated. Sintering was performed at 900 degrees C at a heating rate of 30 degrees C/min for 10 min and under a pressure of 70 MPa. The density of the sintered composite samples was measured by the Archimedes method. A wear test was performed by a ball-on-disc tribometer under dry conditions at room temperature in air. The presence of graphite effectively reduced the wear of composites. The copper-graphite nanocomposites prepared by EEW had lower wear rates than pure copper material and simple mixed copper-graphite.

  18. Measurement and investigation of effects of coal tar pitch fractions in nuclear graphite properties

    International Nuclear Information System (INIS)

    Fatemi, K.; Fatoorehchian, S.; Ahari Hashemi, F.; Ahmadi, Sh.

    2003-01-01

    Coal tar pitch has a complex chemical structure. Determination of α, β, γ fractions, is one of the methods to get information about its properties. In graphite fabrication it plays a role as a binder for coke particles. During the thermal treatment it carbonizes and changes to a secondary coke. This has considerable affects on the graphite properties. In this paper, determination of α, β, γ-1 fraction in three different types of pitches have been carried out. Graphite specimens have been fabricated by using these pitches and anisotropy coke in laboratory scale. The graphite properties have been compared with the nuclear graphite prototype. The comparison of the results showed that the density and compression strength are appreciable while the anisotropy factor of properties is about one. The linear thermal expansion in graphite from Iranian pitch had a better, result, where it stands in the nuclear range of usage. As a result, our studies showed that the graphite properties are affected by properties of pitch fractions, where it can be used as a proper sample for the graphite fabrication

  19. 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.

  20. THE FIRST DISCOVERY OF PRESOLAR GRAPHITE GRAINS FROM THE HIGHLY REDUCING QINGZHEN (EH3) METEORITE

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Yuchen; Lin, Yangting; Zhang, Jianchao; Hao, Jialong, E-mail: linyt@mail.iggcas.ac.cn [Key Laboratory of Earth and Planetary Physics, Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing 100029 (China)

    2016-07-10

    Presolar graphite grains have been extensively studied, but are limited in carbonaceous chondrites, particularly in Murchison (CM2) and Orgueil (CI1), which sampled materials from the oxidizing regions in the solar nebula. Here, we report the first discovery of presolar graphite grains from the Qingzhen (EH3) enstatite chondrite which formed under a highly reducing condition. Eighteen presolar graphite grains were identified by C-isotope mapping of the low-density fraction (1.75–1.85 g cm{sup 3}) from Qingzhen acid residue. Another 58 graphite spherules were found in different areas of the same sample mount using a scanning electron microscope and were classified into three morphologies, including cauliflower, onion, and cauliflower–onion. The Raman spectra of these spherules vary from ordered, disordered, and glassy to kerogen-like, suggestive of a wide range of thermal metamorphisms. NanoSIMS analysis of the C- and Si-isotopes of these graphite spherules confirmed 23 presolar grains. The other 35 graphite spherules have no significant isotopic anomalies, but they share similar morphologies and Raman spectra with the presolar ones. Another three grains were identified during NanoSIMS analysis. Of all the 44 presolar graphite grains identified, six grains show {sup 28}Si-excesses, suggestive of supernovae origins, and four grains