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Sample records for graphite arc furnace

  1. Dross treatment in a rotary arc furnace with graphite electrodes

    NASA Astrophysics Data System (ADS)

    Drouet, Michel G.; Handfield, My; Meunier, Jean; Laflamme, Claude B.

    1994-05-01

    Aluminum baths are always covered with a layer of dross resulting from the aluminum surface oxidation. This dross represents 1-10% of the melt and may contain up to 75wt.% aluminum. Since aluminum production is highly energy intensive, dross recycling is very attractive from both energy and economic standpoints. The conventional recycling process using salt rotary furnaces is thermally inefficient and environmentally unacceptable because of the production of salt slags. Hydro-Quebec has developed a new technology using a rotary arc furnace with graphite electrodes. This process provides aluminum recovery rates of 80-90%, using a highly energy efficient, environmentally sound production method.

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

    SciTech Connect

    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

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

    SciTech Connect

    Surma, J.E.; Freeman, C.J.; Powell, T.D.; Cohn, D.R.; Smatlak, D.L.; Thomas, P.; Woskov, P.P.; Hamilton, R.A.; Titus, C.H.; Wittle, J.K.

    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.

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

    SciTech Connect

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

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

    DOEpatents

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

    2002-12-24

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

  6. Method for processing aluminum spent potliner in a graphite electrode arc furnace

    DOEpatents

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

    2002-12-24

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

  7. Improved graphite furnace atomizer

    DOEpatents

    Siemer, D.D.

    1983-05-18

    A graphite furnace atomizer for use in graphite furnace atomic absorption spectroscopy is described wherein the heating elements are affixed near the optical path and away from the point of sample deposition, so that when the sample is volatilized the spectroscopic temperature at the optical path is at least that of the volatilization temperature, whereby analyteconcomitant complex formation is advantageously reduced. The atomizer may be elongated along its axis to increase the distance between the optical path and the sample deposition point. Also, the atomizer may be elongated along the axis of the optical path, whereby its analytical sensitivity is greatly increased.

  8. Induction graphitizing furnace acceptance test report

    NASA Technical Reports Server (NTRS)

    1972-01-01

    The induction furnace was designed to provide the controlled temperature and environment required for the post-cure, carbonization and graphitization processes for the fabrication of a fibrous graphite NERVA nozzle extension. The acceptance testing required six tests and a total operating time of 298 hrs. Low temperature mode operations, 120 to 850 C, were completed in one test run. High temperature mode operations, 120 to 2750 C, were completed during five tests.

  9. Acoustic characteristics of electric arc furnaces

    NASA Astrophysics Data System (ADS)

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

    2016-06-01

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

  10. A rotary arc furnace for aluminum dross processing

    SciTech Connect

    Drouet, M.G.; Meunier, J.; Laflamme, C.B.; Handfield, M.D.; Biscaro, A.; Lemire, C.

    1995-12-31

    Dross, a major by-product of all processes involving molten aluminum, forms at the surface of the molten metal as the latter reacts with the furnace atmosphere. It generally represents 1 to 5 wt% of the melt, depending on the process, and contains on average about 50% free aluminum dispersed in an oxide layer. Since aluminum production is highly energy-intensive, dross recycling is very attractive from both the energy and the economic standpoints. The conventional recycling process using salt rotary furnaces is thermally inefficient and environmentally non-acceptable because of the production of salt slags. Hydro-Quebec has developed and patented a new salt-free technology using a rotary furnace heated by an electric arc between two graphite electrodes, called DROSCAR{reg_sign}. A 600-kW pilot plant in operation at LTEE is in use to demonstrate the process. This process provides aluminum recovery rates over 90%, using a highly energy efficient, environmentally sound production method. In 1994, 400 tonnes of aluminum dross were treated in this facility and several tests on various types of dross have also been conducted in early 1995. A report on the results will be presented.

  11. A rotary arc furnace for aluminum dross processing

    SciTech Connect

    Drouet, M.G.; Meunier, J.; Laflamme, C.B.; Handfield, M.D.; Biscaro, A.; Lemire, C.

    1995-12-31

    Dross, a major by-product of all processes involving molten aluminum, forms at the surface of the molten metal as the latter reacts with the furnace atmosphere. It generally represents 1 to 5 wt% of the melt, depending on the process, and contains on average about 50% free aluminum dispersed in an oxide layer. Since aluminum production is highly energy-intensive, dross recycling is very attractive from both the energy and the economic standpoints. The conventional recycling process using salt rotary furnaces is thermally inefficient and environmentally unacceptable because of the salt slags produced. Hydro-Quebec has developed and patented a new salt-free technology using a rotary furnace heated by an electric arc between two graphite electrodes, called DROSCAR{reg_sign}. A 600-kW pilot plant in operation at LTEE is in use to demonstrate the process. This process provides aluminum recovery rates for over 90%, using a highly energy efficient, environmentally sound production method. In 1994, 400 tons of aluminum dross were treated in this facility and several tests on various types of dross have also been conducted in early 1995. A report on the results will be presented.

  12. TILTING ELECTRIC ARC FURNACE USED TO MELT BRONZE IN THE ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    TILTING ELECTRIC ARC FURNACE USED TO MELT BRONZE IN THE BRASS FOUNDRY BY MEANS OF AN ARC CREATED BETWEEN TWO HORIZONTAL ELECTRODES. WHEN MELTED, THE FURNACE TILTS, FILLING MOBILE LADLES FROM THE SPOUT. - Stockham Pipe & Fittings Company, Brass Foundry, 4000 Tenth Avenue North, Birmingham, Jefferson County, AL

  13. Hydrothermal treatment of electric arc furnace dust.

    PubMed

    Yu, Bing-Sheng; Wang, Yuh-Ruey; Chang, Tien-Chin

    2011-06-15

    In this study, ZnO crystals were fabricated from electric arc furnace dust (EAFD) after alkaline leaching, purification and hydrothermal treatment. The effects of temperature, duration, pH, and solid/liquid ratio on ZnO crystal morphology and size were investigated. Results show a high reaction temperature capable of accelerating the dissolution of ZnO precursor, expediting the growth of 1D ZnO, and increasing the L/D ratio in the temperature range of 100-200°C. ZnO crystals with high purity can also be obtained, using the one-step hydrothermal treatment with a baffle that depends on the different solubility of zincite and franklinite in the hydrothermal conditions. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. Plumbrook Hypersonic Tunnel Facility Graphite Furnace Degradation Mechanisms

    NASA Technical Reports Server (NTRS)

    Jacobson, Nathan S.

    1999-01-01

    A recent rebuild revealed extensive degradation to the large graphite induction furnace in the Hypersonic Tunnel Facility (HTF). This damage to the graphite blocks and insulating felt is examined and modeled with thermochemical equilibrium codes. The primary reactions appear to be with water vapor and the nitrogen purge gas. Based on these conclusions, several changes are recommended. An inert purge gas (e.g. argon or helium) and controlling and monitoring water vapor to about 10 ppm should decrease the damage substantially.

  15. Computational Modeling of Arc-Slag Interaction in DC Furnaces

    NASA Astrophysics Data System (ADS)

    Reynolds, Quinn G.

    2017-02-01

    The plasma arc is central to the operation of the direct-current arc furnace, a unit operation commonly used in high-temperature processing of both primary ores and recycled metals. The arc is a high-velocity, high-temperature jet of ionized gas created and sustained by interactions among the thermal, momentum, and electromagnetic fields resulting from the passage of electric current. In addition to being the primary source of thermal energy, the arc jet also couples mechanically with the bath of molten process material within the furnace, causing substantial splashing and stirring in the region in which it impinges. The arc's interaction with the molten bath inside the furnace is studied through use of a multiphase, multiphysics computational magnetohydrodynamic model developed in the OpenFOAM® framework. Results from the computational solver are compared with empirical correlations that account for arc-slag interaction effects.

  16. Computational Modeling of Arc-Slag Interaction in DC Furnaces

    NASA Astrophysics Data System (ADS)

    Reynolds, Quinn G.

    2016-11-01

    The plasma arc is central to the operation of the direct-current arc furnace, a unit operation commonly used in high-temperature processing of both primary ores and recycled metals. The arc is a high-velocity, high-temperature jet of ionized gas created and sustained by interactions among the thermal, momentum, and electromagnetic fields resulting from the passage of electric current. In addition to being the primary source of thermal energy, the arc jet also couples mechanically with the bath of molten process material within the furnace, causing substantial splashing and stirring in the region in which it impinges. The arc's interaction with the molten bath inside the furnace is studied through use of a multiphase, multiphysics computational magnetohydrodynamic model developed in the OpenFOAM® framework. Results from the computational solver are compared with empirical correlations that account for arc-slag interaction effects.

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

    SciTech Connect

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

    1999-09-01

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

  18. Vitrification of electric arc furnace dusts.

    PubMed

    Pelino, M; Karamanov, A; Pisciella, P; Crisucci, S; Zonetti, D

    2002-01-01

    Electric arc furnace baghouse dust (EAFD), a waste by-product of the steelmaking process, contains the elements that are volatilized from the charge during the melting (Cr, Pb, Zn, Cu and Cd). The results of leaching tests show that the concentration of these elements exceeds the regulatory limits. Consequently, EAFD cannot be disposed of in ordinary landfill sites without stabilization of the heavy metals. In this work, the vitrification of EAFD, from both carbon and stainless steel productions, were studied. The vitrification process was selected as the inertizing process because it permits the immobilization of the hazardous elements in the glass network and represents an environmentally acceptable method for the stabilization of this waste. Classes of various compositions were obtained by mixing EAFD with glass cullet and sand. The EAFD and the glass products were characterized by DTA, TG, X-ray analysis and by the TCLP test. The results show that the stability of the product is influenced by the glass structure, which mainly depends on the Si/O ratio. Secondary crystallization heat-treatment were carried out on some samples. The results highlighted the formation of spinel phases, which reduced the chemical durability in acid media. The possibility to recover Zn from carbon steel production EAFD was investigated and about 60-70% of metal recovery was obtained. The resulting glass show higher chemical stability than glasses obtained without metal recovery.

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

    NASA Astrophysics Data System (ADS)

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

    2017-04-01

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

  20. Rapid analysis with transversely heated graphite furnace atomic absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Li, Zhang; Carnrick, Glen; Slavin, Walter

    1993-09-01

    A new graphite furnace instrument using a transversely heated furnace tube with a longitudinal Zeeman correction system has been specifically designed to provide more nearly stabilized temperature platform furnace (STPF) conditions than previous furnace systems. Because there are no cold ends on this furnace tube on which to condense analyte and matrix materials, the vapor phase interferences are expected to be smaller. Also, the cooldown step can be avoided, thus saving time. This instrument permits the delivery of sample into a furnace already heated. The delivery rate of the autosampler can be slowed. These opportunities make it feasible for the sample to be dry on the platform by the time the delivery is complete. Several elements of environmental significance were chosen for test: As, Pb, Se, Tl, Cd, Cu, Cr and V. In almost all of these situations, the analyte was fully recovered without using a matrix modifier or a pyrolysis step. However, As and Pb in urine and As in sediment required a modifier and pyrolysis step for accurate results. A new fast furnace protocol was developed to accommodate use of a matrix modifier and this new protocol was successful for Pb and As in these matrices. All the procedures required less than 1 min total cycle times and produced results in agreement with certified values. This is in contrast with conventional methods which require 2-3 min per firing. These results confirm that graphite furnace methods can be accomplished with a throughput greater than 60 determinations per hour, and eventually, it may be possible to increase this rate beyond 100 determinations per hour.

  1. DC Arc Furnaces — Past, Present, and Future

    NASA Astrophysics Data System (ADS)

    Jones, Rodney T.

    DC arc furnaces were first used industrially for the reductive smelting of chromite fines to produce ferrochromium thirty years ago. Since then, they have been used for a variety of applications, including the smelting of ilmenite to produce titania slag and pig iron, the recovery of cobalt from non-ferrous smelter slags, and the smelting of nickel laterite ores to produce ferronickel. The power of these furnaces has increased from 12 MW to 72 MW for ferrochromium, and to 80 MW for ferronickel. The largest of these furnaces requires two electrodes to carry sufficient current to generate this much power. A review is presented of various DC arc furnaces in use, along with a discussion of the likely ways in which furnace power might be increased further in the future.

  2. Energy Balance in DC Arc Plasma Melting Furnace

    NASA Astrophysics Data System (ADS)

    Zhao, Peng; Meng, Yuedong; Yu, Xinyao; Chen, Longwei; Jiang, Yiman; Ni, Guohua; Chen, Mingzhou

    2009-04-01

    In order to treat hazardous municipal solid waste incinerator's (MSWI) fly ash, a new DC arc plasma furnace was developed. Taking an arc of 100 V/1000 A DC as an example, the heat transfer characteristics of the DC arc plasma, ablation of electrodes, heat properties of the fly ash during melting, heat transfer characteristics of the flue gas, and heat loss of the furnace were analyzed based on the energy conservation law, so as to achieve the total heat information and energy balance during plasma processing, and to provide a theoretical basis for an optimized design of the structure and to improve energy efficiency.

  3. Structural ceramics containing electric arc furnace dust.

    PubMed

    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

  4. Method of operating a centrifugal plasma arc furnace

    DOEpatents

    Kujawa, Stephan T.; Battleson, Daniel M.; Rademacher, Jr., Edward L.; Cashell, Patrick V.; Filius, Krag D.; Flannery, Philip A.; Whitworth, Clarence G.

    1998-01-01

    A centrifugal plasma arc furnace is used to vitrify contaminated soils and other waste materials. An assessment of the characteristics of the waste is performed prior to introducing the waste into the furnace. Based on the assessment, a predetermined amount of iron is added to each batch of waste. The waste is melted in an oxidizing atmosphere into a slag. The added iron is oxidized into Fe.sub.3 O.sub.4. Time of exposure to oxygen is controlled so that the iron does not oxidize into Fe.sub.2 O.sub.3. Slag in the furnace remains relatively non-viscous and consequently it pours out of the furnace readily. Cooled and solidified slag produced by the furnace is very resistant to groundwater leaching. The slag can be safely buried in the earth without fear of contaminating groundwater.

  5. Method of operating a centrifugal plasma arc furnace

    DOEpatents

    Kujawa, S.T.; Battleson, D.M.; Rademacher, E.L. Jr.; Cashell, P.V.; Filius, K.D.; Flannery, P.A.; Whitworth, C.G.

    1998-03-24

    A centrifugal plasma arc furnace is used to vitrify contaminated soils and other waste materials. An assessment of the characteristics of the waste is performed prior to introducing the waste into the furnace. Based on the assessment, a predetermined amount of iron is added to each batch of waste. The waste is melted in an oxidizing atmosphere into a slag. The added iron is oxidized into Fe{sub 3}O{sub 4}. Time of exposure to oxygen is controlled so that the iron does not oxidize into Fe{sub 2}O{sub 3}. Slag in the furnace remains relatively non-viscous and consequently it pours out of the furnace readily. Cooled and solidified slag produced by the furnace is very resistant to groundwater leaching. The slag can be safely buried in the earth without fear of contaminating groundwater. 3 figs.

  6. Temperature field in Graphite-Silicon-Graphite samples heated in monoellipsoidal mirror furnaces

    NASA Astrophysics Data System (ADS)

    Rivas, Damián; Haya, Rodrigo

    1999-01-01

    The heating of cylindrical compound samples in monoellipsoidal mirror furnaces is analyzed by means of a conduction-radiation model that includes the radiative exchange between the sample and the mirror, and that takes into account the temperature dependence of the physical properties of the materials that form the sample. Graphite-Silicon-Graphite samples are considered. The melting of the Silicon part, and the temperature difference between the two Graphite rods that hold the Silicon melt zone are analyzed. The relative position of the Silicon part in the compound sample turns out to be a very sensitive parameter: it affects (1) the power needed to melt the Silicon zone, and (2) the temperature difference between the solid Graphite rods.

  7. Temporal variation in gas temperature at the atomization stage in several types of graphite furnaces for atomic absorption spectrometry.

    PubMed

    Ashino, Tetsuya; Shimabukuro, Haruki; Morimoto, Shun; Wagatsuma, Kazuaki

    2009-10-01

    In order to compare and evaluate the atomization process occurring in several types of graphite furnaces for atomic absorption spectrometry, the authors estimated temporal variations in the gas temperature by using a two-line method under the assumption of a Bolzmann distribution. The atomization furnaces employed were a graphite tube, a graphite tube coated with pyrolitic carbon, a graphite tube with a platform and a graphite cup. Differences in the temporal variation in the gas temperature among these graphite furnaces were observed.

  8. Studies of atomization from a graphite platform in graphite-furnace atomic-absorption spectrometry.

    PubMed

    Chakrabarti, C L; Chang, S B; Thong, P W; Huston, T J; Wu, S

    1987-02-01

    A theoretical model has been proposed for the transient characteristics of an atomic-absorption pulse generated by atomization from a graphite platform in a pulse-heated graphite-furnace atomic-absorption spectrometer. The model has been used (with the aid of a computer program) to predict the effects of various factors on analyte atom populations as a function of time. The various factors studied were heating rate, initial temperature of the graphite tube wall, platform mass and thickness, and activation energy for the rate-determining step in the reaction sequence leading to atom formation. The results predicted by the model are in reasonable agreement with the experimental results obtained by using lead as the analyte element.

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

    PubMed

    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).

  10. GUI for studying the parameters influence of the electric arc model for a three-phase electric arc furnace

    NASA Astrophysics Data System (ADS)

    Ghiormez, L.; Prostean, O.; Panoiu, M.; Panoiu, C.

    2017-01-01

    This paper presents an analysis regarding the modeling of the behavior for a three-phase electric arc furnace installation. Therefore, a block diagram is implemented in Simulink that represents the modeling of the entire electric arc furnace installation. This block diagram contains also the modeling of the electric arc which is the element that makes the electric arc furnace behaving as a nonlinear load. The values for the model parameters of the electric arc furnace installation are like the ones from the real installation taken into consideration. Other model parameters are the electric arc model ones. In order to study the influence of the parameters of the electric arc models, it is developed a Matlab program that contains the graphical user interfaces. These interfaces make connection with the models of the electric arc implemented in Simulink. The interfaces allow the user to modify parameters for each of the electric arc model. Current and voltage of the electric arc are the variables taken into account to study the influence of the parameters on the electric arc models. Waveforms for voltage and current of the electric arc are illustrated when a parameter of the model is modified in order to analyze the importance of this parameter on the electric arc model. Also, for each of the models is presented the voltage-current characteristic of the electric arc because this characteristic gives information about the behavior of the electric arc furnace installation.

  11. Characterization of Sintering Dust, Blast Furnace Dust and Carbon Steel Electric Arc Furnace Dust

    NASA Astrophysics Data System (ADS)

    Chang, Feng; Wu, Shengli; Zhang, Fengjie; Lu, Hua; Du, Kaiping

    In order to make a complete understanding of steel plant metallurgical dusts and to realize the goal of zero-waste, a study of their properties was undertaken. For these purposes, samples of two sintering dusts (SD), two blast furnace dusts (BFD), and one electric arc furnace dust (EAFD) taken from the regular production process were subjected to a series of tests. The tests were carried out by using granulometry analysis, chemical analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy via SEM (EDS), and Fourier transform infrared spectroscopy (FTIR). The dominant elements having an advantage of reuse are Fe, K, Cl, Zn, C. The dominant mineralogical phases identified in sintering dust are KCl, Fe2O3, CaCO3, CaMg(CO3)2, NaCl, SiO2. Mineralogical phases exist in blast furnace dust are Fe2O3, Fe3O4, with small amount of KCl and kaolinite coexist. While in electric arc furnace dust, Fe3O4, ZnFe2O4, CaCO3, CaO, Ca(OH)2 are detected.

  12. High-bandwidth continuous-flow arc furnace

    DOEpatents

    Hardt, David E.; Lee, Steven G.

    1996-01-01

    A high-bandwidth continuous-flow arc furnace for stream welding applications includes a metal mass contained in a crucible having an orifice. A power source charges an electrode for generating an arc between the electrode and the mass. The arc heats the metal mass to a molten state. A pressurized gas source propels the molten metal mass through the crucible orifice in a continuous stream. As the metal is ejected, a metal feeder replenishes the molten metal bath. A control system regulates the electrode current, shielding gas pressure, and metal source to provide a continuous flow of molten metal at the crucible orifice. Independent control over the electrode current and shield gas pressure decouples the metal flow temperature and the molten metal flow rate, improving control over resultant weld characteristics.

  13. High-bandwidth continuous-flow arc furnace

    DOEpatents

    Hardt, D.E.; Lee, S.G.

    1996-08-06

    A high-bandwidth continuous-flow arc furnace for stream welding applications includes a metal mass contained in a crucible having an orifice. A power source charges an electrode for generating an arc between the electrode and the mass. The arc heats the metal mass to a molten state. A pressurized gas source propels the molten metal mass through the crucible orifice in a continuous stream. As the metal is ejected, a metal feeder replenishes the molten metal bath. A control system regulates the electrode current, shielding gas pressure, and metal source to provide a continuous flow of molten metal at the crucible orifice. Independent control over the electrode current and shield gas pressure decouples the metal flow temperature and the molten metal flow rate, improving control over resultant weld characteristics. 4 figs.

  14. Modeling of Thermal Phenomena and Economic Aspect of Configuring Furnace Graphite Insulation

    NASA Astrophysics Data System (ADS)

    Sawicki, J.; Gutkowski, A.; Kaczmarek, I.; Paweta, S.; Rylski, A.

    2015-03-01

    The effect of long-term heating on the graphite thermal insulation of a chamber furnace is considered. Mathematical modeling of the process is performed with the help of the ANSYS-FLUENT software. The formation of surface layers is analyzed from the standpoint of economy by comparing furnaces with advanced configuration of the thermal insulation and with the traditional thermal insulation of chamber furnaces. The configuration of the graphite thermal insulation of a furnace is optimized in terms of the heat treatment cost.

  15. Diagnostics for a waste processing plasma arc furnace (invited) (abstract)a)

    NASA Astrophysics Data System (ADS)

    Woskov, P. P.

    1995-01-01

    Maintaining the quality of our environment has become an important goal of society. As part of this goal new technologies are being sought to clean up hazardous waste sites and to treat ongoing waste streams. A 1 MW pilot scale dc graphite electrode plasma arc furnace (Mark II) has been constructed at MIT under a joint program among Pacific Northwest Laboratory (PNL), MIT, and Electro-Pyrolysis, Inc. (EPI)c) for the remediation of buried wastes in the DOE complex. A key part of this program is the development of new and improved diagnostics to study, monitor, and control the entire waste remediation process for the optimization of this technology and to safeguard the environment. Continuous, real time diagnostics are needed for a variety of the waste process parameters. These parameters include internal furnace temperatures, slag fill levels, trace metals content in the off-gas stream, off-gas molecular content, feed and slag characterization, and off-gas particulate size, density, and velocity distributions. Diagnostics are currently being tested at MIT for the first three parameters. An active millimeter-wave radiometer with a novel, rotatable graphite waveguide/mirror antenna system has been implemented on Mark II for the measurement of surface emission and emissivity which can be used to determine internal furnace temperatures and fill levels. A microwave torch plasma is being evaluated for use as a excitation source in the furnace off-gas stream for continuous atomic emission spectroscopy of trace metals. These diagnostics should find applicability not only to waste remediation, but also to other high temperature processes such as incinerators, power plants, and steel plants.

  16. Glass-ceramic materials from electric arc furnace dust.

    PubMed

    Kavouras, P; Kehagias, T; Tsilika, I; Kaimakamis, G; Chrissafis, K; Kokkou, S; Papadopoulos, D; Karakostas, Th

    2007-01-31

    Electric arc furnace dust (EAFD) was vitrified with SiO2, Na2CO3 and CaCO3 powders in an electric furnace at ambient atmosphere. Vitreous products were transformed into glass-ceramic materials by two-stage heat treatment, at temperatures determined by differential thermal analysis. Both vitreous and glass-ceramic materials were chemically stable. Wollastonite (CaSiO3) was separated from the parent matrix as the dominant crystalline phase, verified by X-ray diffraction analysis and energy dispersive spectrometry. Transmission electron microscopy revealed that wollastonite crystallizes mainly in its monoclinic form. Knoop microhardness was measured with the static indentation test method in all initial vitreous products and the microhardness values were in the region of 5.0-5.5 GPa. Devitrification resulted in glass-ceramic materials with microhardness values strongly dependent on the morphology and orientation of the separated crystal phase.

  17. Effect of the chemical composition of slag on its foamability in an electric arc furnace

    NASA Astrophysics Data System (ADS)

    Kozhukhov, A. A.

    2015-06-01

    The problems of foaming electric furnace slags are considered. The role of the physicochemical properties of slag during its foaming in electric arc furnaces is studied. The regions of slag foaming in an electric arc furnace are determined. Based on the derived relations between the chemical composition of slag and its foamability, one can choose a rational path of slag formation to ensure good slag foaming in the course of electrosmelting of steel.

  18. 40 CFR 63.10686 - What are the requirements for electric arc furnaces and argon-oxygen decarburization vessels?

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Hazardous Air Pollutants for Area Sources: Electric Arc Furnace Steelmaking Facilities Standards and Compliance Requirements § 63.10686 What are the requirements for electric arc furnaces and argon-oxygen... arc furnaces and argon-oxygen decarburization vessels? 63.10686 Section 63.10686 Protection of...

  19. 40 CFR 63.10686 - What are the requirements for electric arc furnaces and argon-oxygen decarburization vessels?

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... Hazardous Air Pollutants for Area Sources: Electric Arc Furnace Steelmaking Facilities Standards and Compliance Requirements § 63.10686 What are the requirements for electric arc furnaces and argon-oxygen... arc furnaces and argon-oxygen decarburization vessels? 63.10686 Section 63.10686 Protection of...

  20. Pragmatic analysis of the electric submerged arc furnace continuum

    PubMed Central

    Karkalos, N.; Xenidis, A.

    2017-01-01

    A transient mathematical model was developed for the description of fluid flow, heat transfer and electromagnetic phenomena involved in the production of ferronickel in electric arc furnaces. The key operating variables considered were the thermal and electrical conductivity of the slag and the shape, immersion depth and applied electric potential of the electrodes. It was established that the principal stimuli of the velocities in the slag bath were the electric potential and immersion depth of the electrodes and the thermal and electrical conductivities of the slag. Additionally, it was determined that, under the set of operating conditions examined, the maximum slag temperature ranged between 1756 and 1825 K, which is in accordance with industrial measurements. Moreover, it was affirmed that contributions to slag stirring due to Lorentz forces and momentum forces due to the release of carbon monoxide bubbles from the electrode surface were negligible.

  1. Modeling of Radiative Heat Transfer in an Electric Arc Furnace

    NASA Astrophysics Data System (ADS)

    Opitz, Florian; Treffinger, Peter; Wöllenstein, Jürgen

    2017-08-01

    Radiation is an important means of heat transfer inside an electric arc furnace (EAF). To gain insight into the complex processes of heat transfer inside the EAF vessel, not only radiation from the surfaces but also emission and absorption of the gas phase and the dust cloud need to be considered. Furthermore, the radiative heat exchange depends on the geometrical configuration which is continuously changing throughout the process. The present paper introduces a system model of the EAF which takes into account the radiative heat transfer between the surfaces and the participating medium. This is attained by the development of a simplified geometrical model, the use of a weighted-sum-of-gray-gases model, and a simplified consideration of dust radiation. The simulation results were compared with the data of real EAF plants available in literature.

  2. Processing electric arc furnace dust into saleable chemical products

    SciTech Connect

    1998-04-01

    The modern steel industry uses electric arc furnace (EAF) technology to manufacture steel. A major drawback of this technology is the production of EAF dust, which is listed by the U.S. Environmental Protection Agency as a hazardous waste under the Resource Conservation and Recovery Act. The annual disposal of approximately 0.65 million tons of EAF dust in the United States and Canada is an expensive, unresolved problem for the steel industry. EAF dust byproducts are generated during the manufacturing process by a variety of mechanisms. The dust consists of various metals (e.g., zinc, lead, cadmium) that occur as vapors at 1,600{degrees}C (EAF hearth temperature); these vapors are condensed and collected in a baghouse. The production of one ton of steel will generate approximately 25 pounds of EAF dust as a byproduct, which is currently disposed of in landfills.

  3. Removal of chloride from electric arc furnace dust.

    PubMed

    Chen, Wei-Sheng; Shen, Yun-Hwei; Tsai, Min-Shing; Chang, Fang-Chih

    2011-06-15

    Electric arc furnace (EAF) dust with high chloride content increases the threat of dioxin emissions and the high chloride content reduces the value of recycled zinc oxide produced by EAF dust recycling plants. This study conducts a number of laboratory experiments to determine the technical feasibility of a new dechlorination method. These methods consist of a series of roasting processes and water washing processes. In the roasting process, EAF dust was heated in a tube furnace to evaluate the parameters of atmospheric conditions, roasting temperature, and roasting time. Results indicate that sulfation roasting is more efficient in reducing chloride content than other roasting processes. The water washing process can totally remove water-soluble chloride at a solid to liquid ratio of 1:10. However, the remaining water-insoluble substance is difficult to dechlorinate. For example, lead chloride forms a hydroxyl-halide (PbOHCl) and lead chloride carbonate (Pb(2)CO(3)Cl(2)) agglutinative matrix that is hard to wash away.

  4. [Determination of trace sodium ion in high purity water by graphite furnace atomic absorption spectrometry].

    PubMed

    Yuan, Xia; Shen, Shi-gang; Sun, Han-wen

    2007-01-01

    The present paper studied on the determination of trace Na+ in high purity water by graphite furnace atom absorption spectrometry. A method of directly on-line concentrating samples in graphite furnace, multiple charging, ashing, then determining once by directly charging into pools of graphite furnace, was set up. The goal of concentrating samples and avoiding contamination as well as raising sensitivity were finally achieved. To prevent the background of purity water and regent in experiment from covering the ion concentration of the sample, the authors prepared the high purity water and regent to meet the requirement of the experiment by electrodialysis in series with distillation and below-boiling-point quartz distillation at pure worktable. Satisfactory results of linearity and detection limit were obtained. The detection limit with this method was 0. 086 microg x L(-1) for Na+. The recovery was 101%-104%.

  5. Electrochemical generation of volatile form of cadmium and its in situ trapping in a graphite furnace

    NASA Astrophysics Data System (ADS)

    Nováková, Eliška; Rychlovský, Petr; Resslerová, Tina; Hraníček, Jakub; Červený, Václav

    2016-03-01

    This publication describes the combination of flow-through electrochemical generation (EcVG) of cadmium volatile form with its in situ trapping in a graphite furnace atomizer. Three cathode materials (Pt, Pb, and Ti) and four potentially suitable electrolytes (HCl, H2SO4, HCOOH and NaCl) were tested. Automated sampling equipment for the graphite furnace atomizer with an untreated fused silica capillary was used for the introduction of the cadmium volatile form into the iridium-treated graphite furnace. The limit of detection (LOD) of the electrochemical Cd volatile form generation with in situ collection was 1.0 ng ml- 1 (concentration LOD) or 1.5 ng (absolute LOD). The efficiency of the method was estimated and discussed. The effect of selected concomitant ions was evaluated and the accuracy of the proposed method was established by determination of the Cd content in the NIST SRM 1643e certified reference material.

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

    PubMed

    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.

  7. Analysis of arc emission spectra of stainless steel electric arc furnace slag affected by fluctuating arc voltage.

    PubMed

    Aula, Matti; Mäkinen, Ari; Fabritius, Timo

    2014-01-01

    Control of chromium oxidation in the electric arc furnace (EAF) is a significant problem in stainless steel production due to variations of the chemical compositions in the EAF charge. One potential method to control chromium oxidation is to analyze the emission spectrum of the electric arc in order to find indicators of rising chromium content in slag. The purpose of this study was to determine if slag composition can be gained by utilizing electric arc emission spectra in the laboratory environment, despite electric arc voltage fluctuations and varying slag composition. The purpose of inducing voltage fluctuation was to simulate changes in the industrial EAF process. The slag samples were obtained from Outokumpu Stainless Oy Tornio Works, and three different arc currents were used. The correlation analysis showed that the emission spectra offer numerous peak ratios with high correlations to the X-ray fluorescence-measured slag CrO(x)/FeO(x) and MnO/SiO2 ratios. These ratios are useful in determining if the reduction agents have been depleted in the EAF. The results suggest that analysis of laboratory-scale electric arc emission spectra is suitable for indicating the high CrO(x) or MnO content of the slag despite the arc fluctuations. Reliable analysis of other slag components was not successful.

  8. New algorithm for controlling electric arc furnaces using their vibrational and acoustic characteristics

    NASA Astrophysics Data System (ADS)

    Cherednichenko, V. S.; Bikeev, R. A.; Serikov, V. A.; Rechkalov, A. V.; Cherednichenko, A. V.

    2016-12-01

    The processes occurring in arc discharges are analyzed as the sources of acoustic radiation in an electric arc furnace (EAF). Acoustic vibrations are shown to transform into mechanical vibrations in the furnace laboratory. The shielding of the acoustic energy fluxes onto water-cooled wall panels by a charge is experimentally studied. It is shown that the rate of charge melting and the depth of submergence of arc discharges in the slag and metal melt can be monitored by measuring the vibrational characteristics of furnaces and using them in a universal industrial process-control system, which was developed for EAFs.

  9. Optimization of anthracite calcination process in a vertical electric arc furnace

    SciTech Connect

    Perron, J.; Bouvette, J.F.; Dupuis, M.

    1996-10-01

    Anthracite is used for cathode block manufacturing must be calcined prior to its use to eliminate volatile matter and reduce its electrical resistivity. Anthracite calcination in vertical electric arc furnaces is widely used in the industry. It is well known that this technology leads to a radial temperature gradient in the furnace which results in non-homogeneous calcined anthracite properties. Also, operation experience has shown that production of calcination furnaces can be difficult to stabilize if process changes occur, which may lead to variable quality of the calcined material. To optimize the calcination process, an improved control strategy and a mathematical model of Elkem-type electric arc furnace were developed. Using these, it was successfully demonstrated that temperature gradient in the furnace can be reduced and that furnace productivity can be substantially increased.

  10. Calculation of gas release from DC and AC arc furnaces in a foundry

    NASA Astrophysics Data System (ADS)

    Krutyanskii, M. M.; Nekhamin, S. M.; Rebikov, E. M.

    2016-12-01

    A procedure for the calculation of gas release from arc furnaces is presented. The procedure is based on the stoichiometric ratios of the oxidation of carbon in liquid iron during the oxidation heat period and the oxidation of iron from a steel charge by oxygen in the period of solid charge melting during the gas exchange of the furnace cavity with the external atmosphere.

  11. 40 CFR Table K-1 to Subpart K of... - Electric Arc Furnace (EAF) CH4 Emission Factors

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 21 2011-07-01 2011-07-01 false Electric Arc Furnace (EAF) CH4.... 98, Subpt. K, Table K-1 Table K-1 to Subpart K of Part 98—Electric Arc Furnace (EAF) CH4 Emission... charging intermittently every minute. b Temperature measured in off-gas channel downstream of the furnace...

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

    EPA Science Inventory

    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...

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

    EPA Science Inventory

    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...

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

    NASA Astrophysics Data System (ADS)

    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.

  15. Combinatorial synthesis of phosphors using arc-imaging furnace

    PubMed Central

    Ishigaki, Tadashi; Toda, Kenji; Yoshimura, Masahiro; Uematsu, Kazuyoshi; Sato, Mineo

    2011-01-01

    We have applied a novel ‘melt synthesis technique’ rather than a conventional solid-state reaction to rapidly synthesize phosphor materials. During a synthesis, the mixture of oxides or their precursors is melted by light pulses (10–60 s) in an arc-imaging furnace on a water-cooled copper hearth to form a globule of 1–5 mm diameter, which is then rapidly cooled by turning off the light. Using this method, we synthesized several phosphor compounds including Y3Al5O12:Ce(YAG) and SrAl2O4:Eu,Dy. Complex phosphor oxides are difficult to produce by conventional solid-state reaction techniques because of the slow reaction rates among solid oxides; as a result, the oxides form homogeneous compounds or solid solutions. On the other hand, melt reactions are very fast (10–60 s) and result in homogeneous compounds owing to rapid diffusion and mixing in the liquid phase. Therefore, melt synthesis techniques are suitable for preparing multi component homogeneous compounds and solid solutions. PMID:27877432

  16. Mineral phases of weathered and recent electric arc furnace dust.

    PubMed

    Martins, Fernanda Machado; dos Reis Neto, José Manoel; da Cunha, Carlos Jorge

    2008-06-15

    A weathered and a recent sample of electric arc furnace dust (EAFD), generated in a southern Brazilian steel industry, were characterized by X-ray fluorescence spectroscopy (XFA), powder X-ray diffraction (XRD), thermogravimetric analysis (TG), scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS) probe and Fourier transform infrared spectroscopy (FTIR). A quantitative phase composition model, that accounts for the observed data and for the physico-chemical conditions of formation, was postulated for each material. One sample, in the form of a wet paste, was collected from the lowest part of a landfill and corresponds to a weathered material whereas the other sample was collected from the top portion of the landfill and corresponds to a recently produced material. The dominant cations present in both samples are iron, zinc and lead with minor amounts of manganese, calcium and silicon. The dominant mineralogical phases identified in both materials are Magnetite, Franklinite and Zincite. The recent sample has Laurionite whereas the weathered sample has Hydrocerussite and Hydrozincite.

  17. Hydrometallurgically recovering zinc from electric arc furnace dusts

    NASA Astrophysics Data System (ADS)

    Antrekowitsch, J.; Antrekowitsch, H.

    2001-12-01

    The increasing use of zinc-containing scrap for steel production has lead to a high zinc content in the electric arc furnace and converter flue dusts. The cost of disposing of this residue is high due to environmental restrictions. Various recycling processes have been developed for these dusts, but most never reached the pilot plant stage and many investigations were stopped because of metallurgical and economical inefficiencies. While pyrometallurgical methods have to deal with high energy consumption, low zinc yield, and valueless residues, hydrometallurgical processes could offer an economical recycling alternative. This paper describes hydrometallurgical methods for recovering zinc from steel industry dust. These methods can be integrated in the primary zinc-winning process or in galvanization. Investigations of sulfuric-acid leaching show high zinc solubility but also a high iron content in the final liquor. As a result, steps for purification are required that cannot be conducted economically. Alternatively, a NaOH leaching gives a satisfying zinc yield and a very low solubility for the iron that remains in the residue.

  18. Evaluation of the graphite electrode arc melter for processing heterogeneous waste

    SciTech Connect

    O'Connor, William K.; Turner, Paul C.; Soelberg, N.R.; Anderson, G.L.

    1996-01-01

    The U.S. Bureau of Mines (USBM) conducted a series of 4 demonstration melting tests in a 3-phase AC graphite electrode arc furnace at its Albany Research Center (ALRC) thermal treatment facility in Albany, Oregon (now part of the U.S. Department of Energy, DOE). The scope of these tests provides a unique opportunity to evaluate a single melting technology regarding its applicability to the treatment of several different heterogeneous mixed wastes. The current system can continuously process combustible-bearing wastes at feedrates to 682 kg/h (1,500 lb/h), continuously tap slag or glass, and intermittently tap metal products, and includes a close-coupled thermal oxidizer and air pollution control system (APCS). The 4 demonstration melting tests were conducted in cooperation with the American Society of Mechanical Engineers (ASME), the Idaho National Engineering Laboratory (INEL), and the Westinghouse Hanford Company (WHC).

  19. Graphite electrode arc melter demonstration Phase 2 test results

    SciTech Connect

    Soelberg, N.R.; Chambers, A.G.; Anderson, G.L.; O`Connor, W.K.; Oden, L.L.; Turner, P.C.

    1996-06-01

    Several U.S. Department of Energy organizations and the U.S. Bureau of Mines have been collaboratively conducting mixed waste treatment process demonstration testing on the near full-scale graphite electrode submerged arc melter system at the Bureau`s Albany (Oregon) Research Center. An initial test series successfully demonstrated arc melter capability for treating surrogate incinerator ash of buried mixed wastes with soil. The conceptual treatment process for that test series assumed that buried waste would be retrieved and incinerated, and that the incinerator ash would be vitrified in an arc melter. This report presents results from a recently completed second series of tests, undertaken to determine the ability of the arc melter system to stably process a wide range of {open_quotes}as-received{close_quotes} heterogeneous solid mixed wastes containing high levels of organics, representative of the wastes buried and stored at the Idaho National Engineering Laboratory (INEL). The Phase 2 demonstration test results indicate that an arc melter system is capable of directly processing these wastes and could enable elimination of an up-front incineration step in the conceptual treatment process.

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

    PubMed

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

    2015-12-01

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

  1. [Application of solid sampling graphite furnace atomic absorption spectrophotometry to mensuration of brain iron content in rats].

    PubMed

    Zhang, Nan; Sheng, Qing-hai; Shi, Zhen-hua; Zhang, Zhi-guo; Duan, Xiang-lin; Chang, Yan-zhong

    2009-04-01

    In the present study, the authors performed the solid sampling and detected the iron levels in cortex, hippocampus and striatum of rat brain by GFAAS. The authors' results showed that there are no remarkable difference between the data obtained by solid sampling graphite furnace atomic absorption and liquid sampling graphite furnace atomic absorption. Compared to liquid sampling graphite furnace atomic absorption, the sample pre-treatment stage was obviously simplified, the cost was reduced significantly, and the time was shortened significantly in the solid sampling GFAAS. This study will be beneficial to the mensuration of iron content in micro-tissue of animal by solid sampling GFASS.

  2. Characterization of steel mill electric-arc furnace dust.

    PubMed

    Sofilić, Tahir; Rastovcan-Mioc, Alenka; Cerjan-Stefanović, Stefica; Novosel-Radović, Vjera; Jenko, Monika

    2004-06-18

    In order to make a complete characterization of electric-arc furnace (EAF) dust, as hazardous industrial waste, and to solve its permanent disposal and/or recovery, bearing in mind both the volumes formed in the Croatian steel industry and experiences of developed industrial countries, a study of its properties was undertaken. For this purpose, samples of EAF dust, taken from the regular production process in the Zeljezara Sisak Steel Mill between December 2000 and December 2001, were subjected to a series of tests. The chemical composition of EAF dust samples was investigated by means of a several different analytical methods. The results from the chemical analysis show that the approximate order of abundance of major elements in EAF dusts is as follows: Fe, Zn, Mn, Ca, Mg, Si, Pb, S, Cr, Cu, Al, C, Ni, Cd, As and Hg. Granular-metric composition of single samples was determined by applying sieve separation. Scanning electron micro-structural examination of EAF dust microstructure was performed and results indicated that all twelve EAF dusts were composed of solid spherical agglomerates with Fe, Zn, Pb, O, Si and Ca as the principal element. The investigation of grain morphology and the mineralogical composition of EAF dust were taken by combination of high resolution Auger electron spectroscopy (HR AES), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction analysis. The analysis of XPS-spectra determined the presence of zinc in the form of ZnO phase and the presence of lead in the form of PbO phase, i.e. PbSO3/PbSO4 forms. The results of the X-ray diffraction phase analysis show that the basis of the examined EAF dust samples is made of a mixture of metal oxides, silicates and sulphates. The metal concentration, anions, pH value and conductivity in water eluates was determined in order to define the influence of EAF dust on the environment.

  3. Thermodynamic Modeling of Zinc Speciation in Electric Arc Furnace Dust

    NASA Astrophysics Data System (ADS)

    Pickles, Chris A.

    2011-04-01

    The remelting of automobile scrap, containing galvanized steel, in an electric arc furnace (EAF) results in the generation of a dust, which contains considerable amounts of zinc and other metals. Typically, the amount of zinc is of significant commercial value, but the recovery of this metal can be hindered by the varied speciation of zinc. The majority of the zinc exists as zincite (ZnO) and zinc ferrite (ZnFe2O4) or ferritic spinels ((Zn x Mn y Fe1-x-y )Fe2O4), but other zinccontaining species such as zinc chloride, zinc hydroxide chlorides, hydrated zinc sulphates and zinc silicates have also been identified. There is a scarcity of research literature on the thermodynamic aspects of the formation of these zinc-containing species, in particular, the minor zinc-containing species. Therefore, in this study, the equilibrium module of HSC Chemistry® 6.1 was utilized to calculate the types and the amounts of the zinc-containing species. The variables studied were: the gas composition, the temperature and the dust composition. At high temperatures, zincite forms via the reaction of zinc vapour with oxygen gas and the zinc-manganese ferrites form as a result of the reaction of iron-manganese particles with zinc vapour and oxygen. At intermediate temperatures, zinc sulphates are produced through the reaction of zinc oxide and sulphur dioxide gas. As room temperature is approached, zinc chlorides and fluorides form by the reaction of zinc oxide with hydrogen chloride and hydrogen fluoride gases, respectively. Zinc silicate likely forms via the high temperature reaction of zinc vapour and oxygen with silica. In the presence of excess water and as room temperature is approached, the zinc sulphates, chlorides and fluorides can become hydrated.

  4. Innovation approaches to controlling the electric regimes of electric arc furnaces

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

    The processes of current passage in an ac electric arc furnace (EAF) are subjected to industrial experiments and mathematical simulation. It is shown that, when a charge is melted, arcs between charge fragments exist in series with main arc discharges, and these arcs influence the stability of the main arc discharges. The measurement of instantaneous currents and voltages allowed us to perform a real-time calculation of the electrical characteristics of a three-phase circuit and to determine the θ parameter, which characterizes the nonlinearity of the circuit segment between electrodes. Based on these studies, we created an advanced system for controlling the electric regime of EAF.

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

    NASA Astrophysics Data System (ADS)

    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.

  6. Optical emission from a small scale model electric arc furnace in 250-600 nm region.

    PubMed

    Mäkinen, A; Niskanen, J; Tikkala, H; Aksela, H

    2013-04-01

    Optical emission spectroscopy has been for long proposed for monitoring and studying industrial steel making processes. Whereas the radiative decay of thermal excitations is always taking place in high temperatures needed in steel production, one of the most promising environment for such studies are electric arc furnaces, creating plasma in excited electronic states that relax with intense characteristic emission in the optical regime. Unfortunately, large industrial scale electric arc furnaces also present a challenging environment for optical emission studies and application of the method is not straightforward. To study the usability of optical emission spectroscopy in real electric arc furnaces, we have developed a laboratory scale DC electric arc furnace presented in this paper. With the setup, optical emission spectra of Fe, Cr, Cr2O3, Ni, SiO2, Al2O3, CaO, and MgO were recorded in the wavelength range 250-600 nm and the results were analyzed with the help of reference data. The work demonstrates that using characteristic optical emission, obtaining in situ chemical information from oscillating plasma of electric arc furnaces is indeed possible. In spite of complications, the method could possibly be applied to industrial scale steel making process in order to improve its efficiency.

  7. Optical emission from a small scale model electric arc furnace in 250-600 nm region

    SciTech Connect

    Maekinen, A.; Tikkala, H.; Aksela, H.; Niskanen, J.

    2013-04-15

    Optical emission spectroscopy has been for long proposed for monitoring and studying industrial steel making processes. Whereas the radiative decay of thermal excitations is always taking place in high temperatures needed in steel production, one of the most promising environment for such studies are electric arc furnaces, creating plasma in excited electronic states that relax with intense characteristic emission in the optical regime. Unfortunately, large industrial scale electric arc furnaces also present a challenging environment for optical emission studies and application of the method is not straightforward. To study the usability of optical emission spectroscopy in real electric arc furnaces, we have developed a laboratory scale DC electric arc furnace presented in this paper. With the setup, optical emission spectra of Fe, Cr, Cr{sub 2}O{sub 3}, Ni, SiO{sub 2}, Al{sub 2}O{sub 3}, CaO, and MgO were recorded in the wavelength range 250-600 nm and the results were analyzed with the help of reference data. The work demonstrates that using characteristic optical emission, obtaining in situ chemical information from oscillating plasma of electric arc furnaces is indeed possible. In spite of complications, the method could possibly be applied to industrial scale steel making process in order to improve its efficiency.

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

    EPA Science Inventory

    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.

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

    EPA Science Inventory

    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.

  10. Analysis of lithium in deep basalt groundwaters using graphite furnace atomic absorption spectrophotometry

    SciTech Connect

    Dill, J.A.; Marcy, A.D.

    1986-05-01

    Lithium is under consideration for use as a reactive (sorptive) tracer in experiments designed to provide information regarding natural attenuation processes in a basalt-groundwater environment. In support of these activities, background lithium concentrations in samples obtained from a variety of test horizons have been determined using graphite furnace atomic absorption spectrophotometry. Significant interference was observed in these determinations and was found to be due to the presence of silicate in the samples. It was found that these problems could be circumvented through the use of alkaline silicate or synthetic groundwater matrix modifiers. This matrix effect was examined in some detail. Results obtained using the graphite furnace were compared to results obtained using inductively coupled plasma atomic emission spectroscopy.

  11. Atmospheric pressure arc discharge with ablating graphite anode

    SciTech Connect

    Nemchinsky, V. A.; Raitses, Y.

    2015-05-18

    The anodic carbon arc discharge is used to produce carbon nanoparticles. Recent experiments with the carbon arc at atmospheric pressure helium demonstrated the enhanced ablation rate for narrow graphite anodes resulting in high deposition rates of carbonaceous products on the copper cathode (Fetterman et al 2008 Carbon 46 1322–6). The proposed model explains these results with interconnected steady-state models of the cathode and the anode processes. When considering cathode functioning, the model predicts circulation of the particles in the near-cathode region: evaporation of the cathode material, ionization of evaporated atoms and molecules in the near-cathode plasma, return of the resulting ions to the cathode, surface recombination of ions and electrons followed again by cathode evaporation etc. In the case of the low anode ablation rate, the ion acceleration in the cathode sheath provides the major cathode heating mechanism. In the case of an intensive anode ablation, an additional cathode heating is due to latent fusion heat of the atomic species evaporated from the anode and depositing at the cathode. Using the experimental arc voltage as the only input discharge parameter, the model allows us to calculate the anode ablation rate. A comparison of the results of calculations with the available experimental data shows reasonable agreement.

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

    USGS Publications Warehouse

    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.

  13. Arc-furnace model for the study of flicker compensation in electrical networks

    SciTech Connect

    Montanari, G.C.; Loggini, M.; Cavallini, A.; Pitti, L. . Istituto di Elettrotecnica Industriale); Zaninelli, D. . Dipt. di Elettrotecnica)

    1994-10-01

    This paper presents an arc-furnace model consisting of non-linear, time varying resistance where two different time-variation laws of arc length are considered. One consists of a periodic, sinusoidal law, the other of a band-limited white-noise law. The arc-furnace model is implemented by EMTP, referring to actual electric-plant configurations. Simulations are reported where the values of flicker sensation and short-term flicker severity, P[sub ST], are determined according to UIE specifications. It results that the model based on sinusoidal time-variation law can be useful for worst-case approximations, while the model using white-noise law is able to fit flicker measurements made in electric plants supplying arc furnaces. The models are used to investigate the effect on flicker compensation of the insertion of series inductors at the supply side of the furnace transformer. It is shown that considerable reduction of P[sub ST] is obtained at the point of common coupling by series inductor installation at constant furnace active power.

  14. Analysis of harmonic and transient phenomena due to operation of a-c arc furnace

    SciTech Connect

    Sarshar, A.; Sharp, M.; Iravani, R.M.

    1995-07-01

    Operation of an a-c electric arc furnace load is associated with the generation of harmonic currents in the frequency range of fractions of Hertz up to approximately 1,000 Hz. The magnitude of these harmonic current components can be high and depends on the diverse operating condition of the system. Exposure of the furnace yard electrical components to overvoltages and overcurrents as a result of current harmonics, produces high electrical and mechanical stresses in the components which, if not accounted for in design, may result in failures. Operating experience with existing electric furnace installations indicates an uncharacteristically high failure rate of components which impose long time system outages and, thereby, reduce product output. A statistical 3-phase model for an arc furnace load in EMTP for time domain simulation studies will be presented. The model is first validated against field measurements and then used to examine the effect of the insertion of series reactors at the supply side of the furnace transformer on the dynamic inrush current associated with furnace transformer switching. It is shown that the insertion of a series reactor will considerably reduce the impact of furnace transformer dynamic inrush current on the filter components. The model is also used to evaluate the actual required design to withstand capabilities of the filter components. Some of the shortcomings of the conventional specifications are illustrated.

  15. 40 CFR Table K-1 to Subpart K of... - Electric Arc Furnace (EAF) CH4 Emission Factors

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 21 2014-07-01 2014-07-01 false Electric Arc Furnace (EAF) CH4.... 98, Subpt. K, Table K-1 Table K-1 to Subpart K of Part 98—Electric Arc Furnace (EAF) CH4 Emission... charging intermittently every minute. b Temperature measured in off-gas channel downstream of the...

  16. 40 CFR Table K-1 to Subpart K of... - Electric Arc Furnace (EAF) CH4 Emission Factors

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 22 2012-07-01 2012-07-01 false Electric Arc Furnace (EAF) CH4.... 98, Subpt. K, Table K-1 Table K-1 to Subpart K of Part 98—Electric Arc Furnace (EAF) CH4 Emission... charging intermittently every minute. b Temperature measured in off-gas channel downstream of the...

  17. 40 CFR Table K-1 to Subpart K of... - Electric Arc Furnace (EAF) CH4 Emission Factors

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 22 2013-07-01 2013-07-01 false Electric Arc Furnace (EAF) CH4.... 98, Subpt. K, Table K-1 Table K-1 to Subpart K of Part 98—Electric Arc Furnace (EAF) CH4 Emission... charging intermittently every minute. b Temperature measured in off-gas channel downstream of the...

  18. 40 CFR 63.10686 - What are the requirements for electric arc furnaces and argon-oxygen decarburization vessels?

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... arc furnaces and argon-oxygen decarburization vessels? 63.10686 Section 63.10686 Protection of... Compliance Requirements § 63.10686 What are the requirements for electric arc furnaces and argon-oxygen... from each EAF (including charging, melting, and tapping operations) and argon-oxygen decarburization...

  19. 40 CFR 63.10686 - What are the requirements for electric arc furnaces and argon-oxygen decarburization vessels?

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... arc furnaces and argon-oxygen decarburization vessels? 63.10686 Section 63.10686 Protection of... Compliance Requirements § 63.10686 What are the requirements for electric arc furnaces and argon-oxygen... from each EAF (including charging, melting, and tapping operations) and argon-oxygen decarburization...

  20. 40 CFR 63.10686 - What are the requirements for electric arc furnaces and argon-oxygen decarburization vessels?

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... arc furnaces and argon-oxygen decarburization vessels? 63.10686 Section 63.10686 Protection of... Compliance Requirements § 63.10686 What are the requirements for electric arc furnaces and argon-oxygen... from each EAF (including charging, melting, and tapping operations) and argon-oxygen...

  1. Characteristics of electric arc furnaces powered by a low-frequency alternating current

    NASA Astrophysics Data System (ADS)

    Mironov, Yu. M.; Mironova, A. N.

    2016-06-01

    The changes in the parameters of a DSP-100 electric arc furnace that are induced by a decrease in the current frequency are considered. It is shown that the related decrease in the current lead resistances causes an increase in the arc power and voltage, a decrease in the reactive power, and an increase in the electrical efficiency and the power coefficient. The heat indices are expected to be significantly improved.

  2. Multivariate economic performance assessment of an MPC controlled electric arc furnace.

    PubMed

    Wei, Donghui; Craig, Ian K; Bauer, Margret

    2007-06-01

    Economic performance is very important to advanced process control projects investigating whether the investment of control technology is worthwhile. In this paper economic performance assessment of a simulated electric arc furnace is conducted. The dependence of controlled variables and the corresponding economic impact are highlighted.

  3. Valorization of electric arc furnace primary steelmaking slags for cement applications.

    PubMed

    Kim, Hyung-Seok; Kim, Kee-Seok; Jung, Sung Suk; Hwang, Jin Ill; Choi, Jae-Seok; Sohn, Il

    2015-07-01

    To produce supplementary cementitious materials from electric arc furnace (EAF) slags, FeO was reduced using a two-stage reduction process that included an Al-dross reduction reaction followed by direct carbon reduction. A decrease in FeO was observed on tapping after the first-stage reduction, and further reduction with a stirred carbon rod in the second-stage reduction resulted in final FeO content below 5wt%, which is compatible with cement clinker applications. The reduced electric arc furnace slags (REAFS) mixed with cement at a unit ratio exhibited physical properties comparable to those of commercialized ground granulated blast furnace slags (GGBFS). Confocal laser scanning microscopy (CLSM) was used to obtain fundamental information on the cooling characteristics and conditions required to obtain amorphous REAFS. REAFS can be applied in cement mixtures to achieve the hydraulic properties needed for commercial use.

  4. Skid resistance performance of asphalt wearing courses with electric arc furnace slag aggregates.

    PubMed

    Kehagia, Fotini

    2009-05-01

    Metallurgical slags are by-products of the iron and steel industry and are subdivided into blast furnace slag and steel slag according to the different steel-producing processes. In Greece, slags are mostly produced from steelmaking using the electric arc furnace process, and subsequently are either disposed in a random way or utilized by the cement industry. Steel slag has been recently used, worldwide, as hard aggregates in wearing courses in order to improve the skidding resistance of asphalt pavements. At the Highway Laboratory, Department of Civil Engineering of Aristotle University of Thessaloniki research has been carried out in the field of steel slags, and especially in electric arc furnace (EAF) slag, to evaluate their possible use in highway engineering. In this paper, the recent results of anti-skidding performance of steel slag aggregates in highway pavements are presented.

  5. Covalent functionalization of polyhedral graphitic particles synthesized by arc discharge from graphite.

    PubMed

    Voss, E; Vigolo, B; Medjahdi, G; Hérold, C; Marêché, J-F; Ghanbaja, J; Le Normand, F; Mamane, V

    2017-02-15

    Carbon materials including carbon nanoparticles, such as nanographite, graphene and graphenic materials, and carbon nanotubes are known to be highly hydrophobic. Oxidation treatments are widely used as the best methods to improve their affinity in a liquid medium or a polymer matrix so that they can be dispersed, handled and processed. Here, we have applied eight different oxidation treatments in order to graft oxygen-containing functional groups at the surface of polyhedral graphitic particles synthesized by arc discharge from graphite, also called astralenes. The used functionalization approaches include both standard chemical attack by strong oxidants and radical functionalization of the sp(2) network by direct C[double bond, length as m-dash]C bond opening. Commonly efficient functionalization methods were unsuccessful to functionalize astralenes while radicals generated from arylhydrazine could lead to functionalization of the outer surface of astralenes. The occurrence of functionalization could be shown by TGA coupled with MS and XPS. The reported method represents the first example of functionalization of astralenes. The efficiency of the applied functionalization methods is discussed considering the chemical reactivity of different carbon nanomaterials including graphene and carbon nanotubes.

  6. Dissipation of Electrical Energy in Submerged Arc Furnaces Producing Silicomanganese and High-Carbon Ferromanganese

    NASA Astrophysics Data System (ADS)

    Steenkamp, Joalet Dalene; Hockaday, Christopher James; Gous, Johan Petrus; Nzima, Thabo Witness

    2017-09-01

    Submerged-arc furnace technology is applied in the primary production of ferroalloys. Electrical energy is dissipated to the process via a combination of arcing and resistive heating. In processes where a crater forms between the charge zone and the reaction zone, electrical energy is dissipated mainly through arcing, e.g., in coke-bed based processes, through resistive heating. Plant-based measurements from a device called "Arcmon" indicated that in silicomanganese (SiMn) production, at times up to 15% of the electrical energy used is transferred by arcing, 30% in high-carbon ferromanganese (HCFeMn) production, compared with 5% in ferrochromium and 60% in ferrosilicon production. On average, the arcing is much less at 3% in SiMn and 5% in HCFeMn production.

  7. Dissipation of Electrical Energy in Submerged Arc Furnaces Producing Silicomanganese and High-Carbon Ferromanganese

    NASA Astrophysics Data System (ADS)

    Steenkamp, Joalet Dalene; Hockaday, Christopher James; Gous, Johan Petrus; Nzima, Thabo Witness

    2017-06-01

    Submerged-arc furnace technology is applied in the primary production of ferroalloys. Electrical energy is dissipated to the process via a combination of arcing and resistive heating. In processes where a crater forms between the charge zone and the reaction zone, electrical energy is dissipated mainly through arcing, e.g., in coke-bed based processes, through resistive heating. Plant-based measurements from a device called "Arcmon" indicated that in silicomanganese (SiMn) production, at times up to 15% of the electrical energy used is transferred by arcing, 30% in high-carbon ferromanganese (HCFeMn) production, compared with 5% in ferrochromium and 60% in ferrosilicon production. On average, the arcing is much less at 3% in SiMn and 5% in HCFeMn production.

  8. Determination of beryllium in urine by graphite furnace atomic absorption spectrophotometry

    SciTech Connect

    Thorat, D.D.; Bhat, P.N.; Mahadevan, T.N.

    1995-08-01

    A method for the determination of beryllium in urine samples by Graphite Furnace Atomic Absorption Spectrophotometry (GFAAS) has been developed. The background correction problem due to the sample matrix was overcome by solvent extraction step. Urine samples were digested with a mixture of concentrated nitric and sulphuric acids. Beryllium in solution was complexed with acetylacetone, extracted in chloroform at pH 8.5 and back extracted in 2%(v/v) nitric acid for final analysis by AAS. The range of concentrations of beryllium observed in urine samples covering both occupational and control subject was 0.03 - 0.37 ng Be/ml.

  9. Aluminum determined in plasma and urine by atomic absorption spectroscopy with a transversely heated graphite atomizer furnace.

    PubMed

    Bradley, C; Leung, F Y

    1994-03-01

    We compared a stabilized-temperature L'vov platform furnace containing an end-heated graphite atomizer (HGA) and transverse Zeeman background-correction system with a side-heated furnace system (transversely heated graphite atomizer; THGA) containing a longitudinal Zeeman background-correction system for the determination of aluminum in plasma and urine. The regression statistics for the correlation analysis of the two systems (slope coefficient = 0.995, intercept = -1.710, Sy/x = 0.021 micrograms/L) indicate that the systems generate comparable results. The newer technology of the THGA furnace with its more uniform and faster heating cycle allows a lower atomization temperature for aluminum, 2200 degrees C. Analyte carryover was significantly reduced in the THGA furnace system. The THGA system generates results equivalent to HGA in about one-third less time, thus making possible a greater throughput of samples in a busy laboratory.

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

    PubMed

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

    2015-08-01

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

  11. Submerged arc furnace process superior to the Waelz process in reducing PCDD/F emission during thermal treatment of electric arc furnace dust.

    PubMed

    Xu, Fu-Qian; Huang, Shao-Bin; Liao, Wei-Tung; Wang, Lin-Chi; Chang, Yu-Cheng; Chang-Chien, Guo-Ping

    2014-01-01

    Besides the Waelz process, the submerged arc furnace (SAF) process has also been extensively used to retain metals from ashes and scraps in the metallurgical industry. However, very little is known about the formation and depletion of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) from this thermal process. In this study, an electric arc furnace (EAF) dust treatment plant adopting the SAF process was investigated and compared to the plant adopting the Waelz process. The predominant contributor of PCDD/F I-TEQ input was the EAF dusts, accounting for 98.4% of the total. The PCDD/F contents in the generated fly ashes of the SAF were extremely low, as almost all the organic compounds for PCDD/F formation were decomposed by the high operating temperatures (1500-1700 °C) of the SAF. Therefore, the PCDD/F emission factor of the SAF process (46.9 μg I-TEQ/tonne-EAF dust) was significantly lower than that of the Waelz process (840-1120 μg I-TEQ/tonne-EAF dust). Its PCDD/F output/input ratios (0.23 and 0.50 based on mass and toxicity) were also lower than those of the Waelz process plant (0.62 and 1.19). Therefore, the SAF process is superior to the Waelz process in reducing the potential of PCDD/F formation. © 2013.

  12. [Flow of high-voltage current in coal electrodes of arc furnaces as a source of noise of special nature].

    PubMed

    Polanowska, R

    1984-01-01

    The noise level for working arc furnace has been measured. Arc furnaces were found to be the source of infrasounds and acoustic field. The sound pressure levels for infrasounds range from 55 to 77 dB. It has been showed that particular noise level includes the onethird-octave band with middle frequency 100 Hz. The sound pressure levels in this band range from 105 to 110 dB.

  13. Waste form development for a DC arc furnace

    SciTech Connect

    Feng, X.; Bloomer, P.E.; Chantaraprachoom, N.; Gong, M.; Lamar, D.A.

    1996-09-01

    A laboratory crucible study was conducted to develop waste forms to treat nonradioactive simulated {sup 238}Pu heterogeneous debris waste from Savannah River, metal waste from the Idaho National Engineering Laboratory (INEL), and nominal waste also from INEL using DC arc melting. The preliminary results showed that the different waste form compositions had vastly different responses for each processing effect. The reducing condition of DC arc melting had no significant effects on the durability of some waste forms while it decreased the waste form durability from 300 to 700% for other waste forms, which resulted in the failure of some TCLP tests. The right formulations of waste can benefit from devitrification and showed an increase in durability by 40%. Some formulations showed no devitrification effects while others decreased durability by 200%. Increased waste loading also affected waste form behavior, decreasing durability for one waste, increasing durability by 240% for another, and showing no effect for the third waste. All of these responses to the processing and composition variations were dictated by the fundamental glass chemistry and can be adjusted to achieve maximal waste loading, acceptable durability, and desired processing characteristics if each waste formulation is designed for the result according to the glass chemistry.

  14. Recovering aluminum from aluminum dross in a DC electric-arc rotary furnace

    NASA Astrophysics Data System (ADS)

    Tzonev, Tz.; Lucheva, B.

    2007-11-01

    The recycling of aluminum scrap and dross yields significant economic and energy savings, as well environmental benefits. The recovery of aluminum depends on many factors. The aim of this work is to experimentally investigate aluminum recovery under different conditions. In this study, aluminum dross was processed in a direct-current electric-arc rotary furnace. The presence of crushing refractory bodies during processing was found to increase the degree of aluminum recovery by about ten percent.

  15. Wettability of Pyrolytic Graphite by Molten Blast Furnace Slag Bearing TiO2

    NASA Astrophysics Data System (ADS)

    Liu, Yanhui; Lv, Xuewei; Bai, Chenguang; Li, Baohua

    The wettability of graphite by the molten TiO2-CaO-SiO2-Al2O3-MgO (in mass%) Blast Furnace slag has been investigated using the dispensed drop method at 1673 K under the Argon atmosphere (Pressure≈ 1.10 atm). With the increase of TiO2 content in the slag the contact angle rises from 127° up to 147°, meaning that the TiO2 worses the wettability between the molten slag and the graphite. On the contrary, the CaO/SiO2 mass ratio can promote the wettability. Interfacial tensions between the slag and the graphite were also evaluated by using the Young's Equation. Thermodynamics calculations were also carried out to study the interfacial reactions, showing that the reaction sequence agree with the following: reduction of MgO, SiO2, TiO2, boudouard reaction and formation of 2CaO Ti2O3.

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

    NASA Astrophysics Data System (ADS)

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

    2016-12-01

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

  17. High-Purity Composite Briquette for Direct UMG-Si Production in Arc Furnaces

    NASA Astrophysics Data System (ADS)

    Perruchoud, Raymond; Fischer, Jean-Claude

    2013-12-01

    In metallurgical grade Si (MG-Si), the coal (B) and charcoal (P) contents are on average above 30 ppm as the carbon reduction materials used in the arc furnace are either rich in B or in P. A decrease of both impurities by a factor of 3 using purer raw materials would allow for the direct production of the upgraded metallurgical grade (UMG).This would significantly improve the efficiency of the resulting photovoltaic (PV) cells made with the refined solar grade silicon (SoG-Si) or massively decrease the costs of Si purification by shortening the number of steps needed for reaching B and P contents below 1 ppm requested for the SoG-Si used for the PV cells. A composite C/SiO2 briquette fulfilling the purity targets for the direct production of UMG-Si in the arc furnace was developed. The composite contains several carbon materials with different levels of reactivities and quartz sand. The raw materials aspects, the paste and briquette preparation, as well as the final carbonization step are discussed. The finished briquettes are free of volatiles and are mechanically and thermally very stable, thus, ensuring stable arc furnace charges with minimum losses of dust and SiO gas. Semi-industrial trials including the downstream purification steps for the production of SoG-Si by a metallurgical low-cost route are contemplated.

  18. Graphite and ablative material response to CO2 laser, carbon-arc, and xenon-arc radiation

    NASA Technical Reports Server (NTRS)

    Brewer, W. D.

    1976-01-01

    The behavior was investigated of graphite and several charring ablators in a variety of high-radiative heat-flux environments. A commercial-grade graphite and nine state-of-the-art charring ablators were subjected to various radiative environments produced by a CO2 laser and a carbon arc. Graphite was also tested in xenon-arc radiation. Heat-flux levels ranged from 10 to 47 MW/sq m. Tests were conducted in air, nitrogen, helium, and a CO2-N2 mixture which simulated the Venus atmosphere. The experimental results were compared with theoretical results obtained with a one-dimensional charring-ablator analysis and a two-dimensional subliming-ablator analysis. Neither the graphite nor the charring ablators showed significant differences in appearance or microstructure after testing in the different radiative environments. The performance of phenolic nylon and graphite was predicted satisfactorily with existing analyses and published material property data. Good agreement between experimental and analytical results was obtained by using sublimation parameters from a chemical nonequilibrium analysis of graphite sublimation. Some charring ablators performed reasonably well and could withstand radiative fluxes of the level encountered in certain planetary entries. Other materials showed excessive surface recession and/or large amounts of cracking and spalling, and appear to be unsuitable for severe radiative environments.

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

    ERIC Educational Resources Information Center

    Williamson, Mark A.

    1989-01-01

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

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

    ERIC Educational Resources Information Center

    Williamson, Mark A.

    1989-01-01

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

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

    PubMed

    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.

  2. [Determination of trace selenium in edible fungi with graphite furnace atomic absorption spectroscopy].

    PubMed

    Tie, Mei; Zhang, Wei; Li, Jing; Jing, Kui; Zang, Shu-liang; Li, Hua-wei

    2006-01-01

    In the present article, samples were digested by a quartz high-pressure digestion pot, reducing the loss of selenium in digestion. The content of selenium in edible fungi was determined by using graphite furnace atomic absorption spectroscopy, and the results showed that when the content of selenium in edible fungi was determined by using 1% Ni(NO3)2 as a matrix modifier, ashing temperature of 500 degreed C, and atomization temperature of 2 500 degrees C, and rectifying background by deuterium light, the recovery was in the range of 92.1%-115.5%, the relative standard deviation of the method was 1.28%, and the limit of detection was 15.8 microg x L(-1). The method was suitable for the determination of trace selenium in edible fungi with the advantages of being simple, rapid, sensitive, stable and accurate etc., and the results were satisfactory.

  3. Determination of ruthenium in pharmaceutical compounds by graphite furnace atomic absorption spectroscopy.

    PubMed

    Jia, Xiujuan; Wang, Tiebang; Bu, Xiaodong; Tu, Qiang; Spencer, Sandra

    2006-04-11

    A graphite furnace atomic absorption (GFAA) spectrometric method for the determination of ruthenium (Rh) in solid and liquid pharmaceutical compounds has been developed. Samples are dissolved or diluted in dimethyl sulfoxide (DMSO) without any other treatment before they were analyzed by GFAA with a carefully designed heating program to avoid pre-atomization signal loss and to achieve suitable sensitivity. Various inorganic and organic solvents were tested and compared and DMSO was found to be the most suitable. In addition, ruthenium was found to be stable in DMSO for at least 5 days. Spike recoveries ranged from 81 to 100% and the limit of quantitation (LOQ) was determined to be 0.5 microg g(-1) for solid samples or 0.005 microg ml(-1) for liquid samples based a 100-fold dilution. The same set of samples was also analyzed by ICP-MS with a different sample preparation method, and excellent agreement was achieved.

  4. Determination of palladium by graphite furnace atomic absorption spectroscopy without matrix matching.

    PubMed

    Jia, X; Wang, T; Wu, J

    2001-05-30

    A graphite furnace atomic absorption spectroscopy method for the analysis of the palladium (Pd) content in bulk pharmaceutical drug substances and their intermediates prepared in aqueous solutions is extended to samples prepared in acetonitrile (ACN) and ACN-water mixtures as well to samples prepared in dimethyl sulfoxide (DMSO) and DMSO-water mixtures. The Pd content in samples solubilized in these solvents can be accurately determined with calibration established with standards prepared in aqueous solutions without matrix matching or using the method of standard additions. The validity of this method is demonstrated by spike recovery studies and by the agreement with results for the same samples prepared in these solvents, in concentrated nitric acid, and prepared by a microwave digestion system.

  5. Determination of mercury in gold bullion by flame and graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Hinds, Michael W.

    1998-08-01

    A procedure was developed to determine mercury in unrefined gold by flame and graphite furnace atomic absorption spectrometry (FAAS and GFAAS). High acid content (60-80% of concentrated HCl in water) was needed to keep silver (usually present with gold deposits) in solution as a chloro-complex. Although Hg determinations by FAAS and GFAAS have poor sensitivity, the relatively high concentrations of Hg (0.02-0.2%) are well within the capabilities of these techniques. No significant difference was observed between concentration values obtained from these techniques and those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES) with the same sample. The limit of detection (3 s) was found to be approximately 20 μg g -1 for both GFAAS and FAAS determinations. However, FAAS is the recommended method due to simplicity of operation, higher sample throughput, low cost, and ease of method transfer to other laboratories.

  6. Determination of tributyltin in tissues and sediments by graphite furnace atomic absorption spectrometry

    SciTech Connect

    Stephenson, M.D.; Smith, D.R.

    1988-04-01

    A method for the determination of tributyltin (TBT) in tissue and sediments has been developed for environmental samples. The technique involves extraction with methylene chloride and isolation of TBT from mono- and dibutyltin with a sodium hydroxide wash. The TBT is then back extracted and converted to elemental Sn with nitric acid. Analysis is by Zeeman graphite furnace atomic absorption spectrophotometry. Recoveries of spiked samples were between 99% and 111% for mussel and fish tissues and 72% and 99% for various sediments. The limit of quantification was 0.0025 ..mu..g/g for tissue (on a wet weight basis). This technique was developed in response to their need to process large numbers of environmental samples with a minimum time investment.

  7. Determination of lead and cadmium in wines by graphite furnace atomic absorption spectrometry.

    PubMed

    Kim, Meehye

    2004-02-01

    The lead (Pb) and cadmium (Cd) content of various wines on the Korean market were determined by graphite furnace atomic absorption spectrometry using Zeeman background correction and peak area mode. All wine samples were microwave-digested in concentrated HNO(3). Ammonium dihydrogen phosphate and magnesium nitrate were used as matrix modifiers for both Pb and Cd analyses. The mean Pb content of the wines was about 29 microg l(-1) ranging from 5 to 87 microg l(-1). Also, the means of Cd were about 0.5 microg l(-1) ranging from < 0.1 to 3.0 microg l(-1). The mean recoveries of Pb and Cd were 92.8 and 101.3% and their analytical detection limits were 1.0 and 0.1 microg l(-1), respectively. Sixty brands of wine were classified into red and white, but no statistically significant difference in Pb and Cd content was observed.

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

    SciTech Connect

    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.

  9. Thermodynamic modelling of the formation of zinc-manganese ferrite spinel in electric arc furnace dust.

    PubMed

    Pickles, C A

    2010-07-15

    Electric arc furnace dust is generated when automobile scrap, containing galvanized steel, is remelted in an electric arc furnace. This dust is considered as a hazardous waste in most countries. Zinc is a major component of the dust and can be of significant commercial value. Typically, the majority of the zinc exists as zinc oxide (ZnO) and as a zinc-manganese ferrite spinel ((Zn(x)Mn(y)Fe(1-x-y))Fe(2)O(4)). The recovery of the zinc from the dust in metal recycling and recovery processes, particularly in the hydrometallurgical extraction processes, is often hindered by the presence of the mixed ferrite spinel. However, there is a paucity of information available in the literature on the formation of this spinel. Therefore, in the present research, the equilibrium module of HSC Chemistry 6.1 was utilized to investigate the thermodynamics of the formation of the spinel and the effect of variables on the amount and the composition of the mixed ferrite spinel. It is proposed that the mixed ferrite spinel forms due to the reaction of iron-manganese particulates with both gaseous oxygen and zinc, at the high temperatures in the freeboard of the furnace above the steel melt. Based on the thermodynamic predictions, methods are proposed for minimizing the formation of the mixed ferrite spinel. 2010 Elsevier B.V. All rights reserved.

  10. DC Electric Arc Furnace Application for Production of Nickel-Boron Master Alloys

    NASA Astrophysics Data System (ADS)

    Alkan, Murat; Tasyürek, Kerem Can; Bugdayci, Mehmet; Turan, Ahmet; Yücel, Onuralp

    2017-07-01

    In this study, nickel-boron (Ni-B) alloys were produced via a carbothermic reduction starting from boric acid (H3BO3) with high-purity nickel oxide (NiO), charcoal, and wood chips in a direct current arc furnace. In electric arc furnace experiments, different starting mixtures were used, and their effects on the chemical compositions of the final Ni-B alloys were investigated. After the reduction and melting stages, Ni-B alloys were obtained by tapping from the bottom of the furnace. The samples from the designated areas were also taken and analyzed. The chemical composition of the final alloys and selected samples were measured with wet chemical analysis. The Ni-B alloys had a composition of up to 14.82 mass% B. The phase contents of the final alloys and selected samples were measured using x-ray diffraction (XRD). The XRD data helped predict possible reactions and reaction mechanisms. The material and energy balance calculations were made via the XRD Rietveld and chemical compositions. Nickel boride phases started to form 600 mm below the surface. The targeted NiB phase was detected at the tapping zone of the crucible (850-900 mm depth). The energy consumption was 1.84-4.29 kWh/kg, and the electrode consumption was 10-12 g/kg of raw material charged.

  11. DC Electric Arc Furnace Application for Production of Nickel-Boron Master Alloys

    NASA Astrophysics Data System (ADS)

    Alkan, Murat; Tasyürek, Kerem Can; Bugdayci, Mehmet; Turan, Ahmet; Yücel, Onuralp

    2017-09-01

    In this study, nickel-boron (Ni-B) alloys were produced via a carbothermic reduction starting from boric acid (H3BO3) with high-purity nickel oxide (NiO), charcoal, and wood chips in a direct current arc furnace. In electric arc furnace experiments, different starting mixtures were used, and their effects on the chemical compositions of the final Ni-B alloys were investigated. After the reduction and melting stages, Ni-B alloys were obtained by tapping from the bottom of the furnace. The samples from the designated areas were also taken and analyzed. The chemical composition of the final alloys and selected samples were measured with wet chemical analysis. The Ni-B alloys had a composition of up to 14.82 mass% B. The phase contents of the final alloys and selected samples were measured using x-ray diffraction (XRD). The XRD data helped predict possible reactions and reaction mechanisms. The material and energy balance calculations were made via the XRD Rietveld and chemical compositions. Nickel boride phases started to form 600 mm below the surface. The targeted NiB phase was detected at the tapping zone of the crucible (850-900 mm depth). The energy consumption was 1.84-4.29 kWh/kg, and the electrode consumption was 10-12 g/kg of raw material charged.

  12. Liquid phase microextraction and ultratrace determination of cadmium by modified graphite furnace atomic absorption spectrometry.

    PubMed

    Nazari, Saeid

    2009-06-15

    A powerful microextraction technique was used for determination of cadmium in water samples using liquid phase microextraction (LPME) followed by graphite furnace atomic absorption spectrometry (GF-AAS). In a preconcentration step, cadmium was extracted from a 2 ml of its aqueous sample in the pH 7 as 5,7-dibromoquinoline-8-ol (DBQ) complex into a 4 microl drop of benzyl alcohol. After extraction, the micro drop was retracted and directly transferred into a graphite tube modified by [W.Rh.Pd](c). Some effective parameters on extraction and complex formation, such as type and volume of organic solvent, pH, concentration of chelating agent, extraction time and stirring rate were optimized. Under the optimum conditions, the enrichment factor and recovery were 450% and 90%, respectively. The calibration graph was linear in the range of 0.008-1 microg L(-1) with correlation coefficient of 0.9961 under the optimum conditions of the recommended procedure. The detection limit based on the 3Sb criterion was 0.0035 microg L(-1) and relative standard deviation (RSD) for eight replicate measurement of 0.1 microg L(-1) and 0.4 microg L(-1) cadmium was 5.2% and 4.5%, respectively. The characteristic concentration was 0.0032 microg L(-1) equivalent to a characteristic mass of 12.8 fg. In order to evaluate the accuracy and recovery of the presented method the procedure was applied to the analysis of reference materials and seawater.

  13. Determination of lead in table wines by graphite furnace atomic absorption spectrometry.

    PubMed

    Mindak, W R

    1994-01-01

    A quick, easy method was developed for the analysis of table wines for lead quantitated at > or = 14 ng Pb/mL wine. The method uses graphite furnace atomic absorption spectrometry with Zeeman background correction and a L'vov pyrolytic graphite platform. Ammonium dihydrogen phosphate is used as a matrix modifier. Wines are diluted by a factor of 10 with 1% HNO3 and analyzed directly. Their absorbances are compared with those of a standard curve prepared with 1% HNO3. Analytical results obtained by comparison with a standard curve agreed with those obtained by the method of standard additions. Four white, 4 red, and 2 rosé wines were studied. Pb concentrations varied from 15 to 135 ng Pb/mL. Wines fortified with 100 ng Pb/mL had an average recovery of 94%. The average short-term relative standard deviation (RSD) was 2.1%; the average long-term RSD was 7.4%. The estimated detection (3 sigma) and quantitation (10 sigma) limits were 4 and 14 ng Pb/mL, respectively.

  14. Elimination of harmonic induced viable bifurcations with TCSC for ac-fed electric arc furnaces

    NASA Astrophysics Data System (ADS)

    Varan, Metin; Uyarog˜lu, Yılmaz

    2012-11-01

    AC-fed electric arc furnaces (EAFs) are known with their unbalanced, excessively nonlinear and time varying load characteristics. The nonlinear oscillations produced by EAF operation cause several problems to interconnected feed system. Injection of harmonics/interharmonics and rising flicker effects on the feed system are two of major problems produced by EAF. These nonlinear effects result into quasistatic changes in the feed system parameters (L - R) . In last decade many studies have been reported that such quasistatic changes in the feed system parameters result in viable bifurcation formations which strictly cause sudden and drastic changes on system behaviors. This paper presents an analytical control procedure to eliminate viable bifurcation points on L - I and R - I curves that cause sudden resonant peak arc currents. After control procedure, stability margins of EAF are extended into larger levels and viable bifurcation points on the feed system parameter have been eliminated. During study, possible roles of small parameter changes of uncontrolled EAF around bifurcation points and controlled EAF have been traced over time series analysis, phase plane analysis and bifurcation diagrams. A wide collection of useful dynamic analysis procedures for the exploration of studied arc furnace dynamics have been handled through the AUTO open-source algorithms.

  15. Steelworks residues and the Waelz kiln treatment of electric arc furnace dust

    SciTech Connect

    Strohmeier, G.; Bonestell, J.E.

    1996-04-01

    Electric arc furnace dust with a combined zinc and lead content in excess of 20% renders the dumping of this material impossible in many countries, for both statutory and financial reasons. In the Waelz process, dust is treated in a rotary kiln where it is heated to approximately 1,200 C. lead and zinc are volatilized under reducing conditions and collected as fine dust in the off-gas dust collection system. The oxide recovered in the off-gas filters contains approximately 55% Zn and up to 10% Pb, and is ideal feedstock for the Imperial Smelting furnace for lead/zinc recovery. The remaining slag is inert and unleachable so that it can be used as a building aggregate.

  16. Mass and elemental distributions of atmospheric particles nearby blast furnace and electric arc furnace operated industrial areas in Australia.

    PubMed

    Mohiuddin, Kazi; Strezov, Vladimir; Nelson, Peter F; Stelcer, Eduard; Evans, Tim

    2014-07-15

    The improved understanding of mass and elemental distributions of industrial air particles is important due to their heterogeneous atmospheric behaviour and impact on human health and the environment. In this study, particles of different size ranges were collected from three sites in Australia located in the vicinity of iron and steelmaking industries and one urban background site with very little industrial influence. In order to determine the importance of the type of industrial activity on the urban atmospheric quality, the industrial sites selected in this study were in the close proximity to two blast furnace operated and one electric arc furnace based steelmaking sites. The chemical compositions of the collected air particles were analysed using the proton induced X-ray emission (PIXE) technique. This study revealed significantly higher metal concentrations in the atmospheric particles collected in the industrial sites, comparing to the background urban site, demonstrating local influence of the industrial activities to the air quality. The modality types of the particles were found to be variable between the mass and elements, and among elements in the urban and industrial areas indicating that the elemental modal distribution is as important as particle mass for particle pollution modelling. The highest elemental number distribution at all studied sites occurred with particle size of 0.1 μm. Iron was found as the main dominant metal at the industrial atmosphere in each particle size range. The industrial Fe fraction in the submicron and ultrafine size particles was estimated at up to 95% which may be released from high temperature industrial activities with the iron and steelmaking industries being one of the major contributors. Hence, these industrial elemental loadings can highly influence the atmospheric pollution at local urban and regional levels and are required to consider in the atmospheric modelling settings.

  17. The possibility of standardless analysis in graphite furnace atomic absorption spectrometry: determination of gold in geological samples

    NASA Astrophysics Data System (ADS)

    Wei-min, Yang; Zhe-ming, Ni

    1996-01-01

    This paper investigates the possibility of standardless analysis for gold in geological samples using graphite furnace atomic absorption spectrometry. A simplex optimization method is employed to select the optimum experimental conditions for both the conventional and fast furnace programs. The atomization efficiency ( ɛA = 100 × m0(calc)/ m0(exp)) for gold appears to be temperature dependent and is found to be around at 100% at higher atomization temperature. The results show that the standardless determination of gold could be performed in geological samples with the use of palladium as the matrix modifier and the accuracy is better than 7%.

  18. Modifiers and coatings in graphite furnace atomic absorption spectrometry—mechanisms of action (A tutorial review)

    NASA Astrophysics Data System (ADS)

    Ortner, H. M.; Bulska, E.; Rohr, U.; Schlemmer, G.; Weinbruch, S.; Welz, B.

    2002-12-01

    A multitude of different and often contradictory mechanisms for the effects of modifiers and coatings have been proposed. Many of these proposals lack sufficient experimental evidence. Therefore, a series of statements based on our own investigations is given as 'facts'. Another series of statements is made as 'fictions' related to erroneous proposals on the functioning of modifiers and coatings in the pertinent literature. Two basic concepts are developed for the sequence of processes leading to analyte stabilization for the two most important groups of modifiers: refractory carbide forming elements of the IVa-VIa groups of the periodic system on the one hand and Pt-group metals on the other hand. These concepts are based on the main reactions of graphite with elements and compounds: carbide formation and intercalation. Most important experimental results leading to this understanding are described: Penetration measurements for modifiers and analytes indicated the subsurface zone down to approximately 10 μm as the essential place for graphite-analyte-modifier interactions. The reason for this phenomenon is an open porosity of the pyrocarbon coating of 5-10% (v/v) into which liquids penetrate upon sample application. This also indicates that modifiers are best applied by impregnation or electrolysis whereas dense coatings are not advantageous. It is also shown that graphite tube assemblies are dynamic systems with a limited lifetime and carbon losses are an essential feature of tube corrosion. Most frequently found erroneous statements are discussed: (a) Particles on the tube surface are responsible for analyte stabilization and retention during pyrolysis. (b) Analyte stabilization is taking place by formation of intermetallic compounds or thermally stable alloys. (c) Experiments are performed with unrealistic concentrations of analytes and/or modifiers. (d) Dense coatings are advantageous. Finally, a functional schedule is given for the three steps of graphite

  19. Analytical application of 2f-wavelength modulation for isotope selective diode laser graphite furnace atomic absorption spectroscopy.

    PubMed

    Wizemann, H D

    2000-01-01

    Experiences in the analytical application of the 2f-wavelength modulation technique for isotope selective atomic absorption spectroscopy in a graphite furnace are reported. Experimental as well as calculated results are presented, mainly for the natural lithium isotopes. Sensitivity, linearity, and (isotope) selectivity are studied by intensity modulation and wavelength modulation. High selectivities can be attained, however, on the cost of detection power. It is shown that the method enables the measurement of lithium isotope ratios larger than 2000 by absorption in a low-pressure graphite tube atomizer.

  20. Determination of yttrium and rare-earth elements in rocks by graphite-furnace atomic-absorption spectrometry.

    PubMed

    Gupta, J G

    1981-01-01

    With use of synthetic solutions and several international standard reference materials a method has been developed for determining traces of Y, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in rocks by electrothermal atomization in a pyrolytically-coated graphite furnace. Depending on the element, the sensitivity is of the order of 10(-9)-10(-12) g at 2500 degrees . To avoid matrix interferences the lanthanides are separated from the common elements by co-precipitation with calcium and iron as carriers. The data for Canadian reference rock SY-2 (syenite), U.S.G.S. reference rocks W-2 (diabase), DNC-1 (diabase) and BIR-1 (basalt), and South African reference rock NIM-18/69 (carbonatite) obtained by graphite-furnace atomization are compared with the values obtained by flame atomic-absorption. The results are in good agreement with literature values.

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

    NASA Astrophysics Data System (ADS)

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

    2016-12-01

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

  2. Determination of phosphorus using high-resolution diphosphorus molecular absorption spectra produced in the graphite furnace

    NASA Astrophysics Data System (ADS)

    Huang, Mao Dong; Becker-Ross, Helmut; Okruss, Michael; Geisler, Sebastian; Florek, Stefan

    2016-01-01

    Molecular absorption of diphosphorus was produced in a graphite furnace and evaluated in view of its suitability for phosphorus determination. Measurements were performed with two different high-resolution continuum source absorption spectrometers. The first system is a newly in-house developed simultaneous broad-range spectrograph, which was mainly used for recording overview absorption spectra of P2 between 193 nm and 245 nm. The region covers the main part of the C 1Σu+ ← X 1Σg+ electronic transition and shows a complex structure with many vibrational bands, each consisting of a multitude of sharp rotational lines. With the help of molecular data available for P2, an assignment of the vibrational bands was possible and the rotational structure could be compared with simulated spectra. The second system is a commercial sequential continuum source spectrometer, which was used for the basic analytical measurements. The P2 rotational line at 204.205 nm was selected and systematically evaluated with regard to phosphorus determination. The conditions for P2 generation were optimized and it was found that the combination of a ZrC modified graphite tube and borate as a chemical modifier were essential for a good production of P2. Serious interferences were found in the case of nitrate and sulfuric acid, although the nitrate interference can be eliminated by a higher pyrolysis temperature. The reliability of the method was proved by analysis of certified samples. Using standard tubes, a characteristic mass of 10 ng and a limit of detection of 7 ng were found. The values could further be improved by a factor of ten using a miniaturized tube with an internal diameter of 2 mm. Compared to the conventional method based on the phosphorus absorption line at 213.618 nm, the advantages of using P2 are the gentle temperature conditions and the potential of performing a simultaneous multi-line evaluation to further improve the limit of detection.

  3. Properties of steel foundry electric arc furnace dust solidified/stabilized with Portland cement.

    PubMed

    Salihoglu, Guray; Pinarli, Vedat; Salihoglu, Nezih Kamil; Karaca, Gizem

    2007-10-01

    Electric arc furnace dust from steel production is generated in considerable amounts worldwide and needs to be treated as hazardous waste. The aim of this study was to investigate the properties of electric arc furnace dust solidified/stabilized by using Portland cement. Mortar and paste samples were prepared with varying waste-to-binder ratios between 0% and 90%. A comprehensive experimental program was designed including XRF characterization, setting time, unconfined compressive strength, and toxicity characteristics leaching procedure (TCLP), synthetic precipitation leaching procedure (SPLP), and acid neutralization capacity (ANC) tests. The results were evaluated in order to determine if the solidified /stabilized product can be disposed of at a landfill site with domestic waste or at a segregated landfill. The effect of using sand on S/S performance was also investigated. The results indicated that the solidification /stabilization process using PC helps the heavy metals to be bound in the cement matrix, but the TCLP leaching results exceeded the EPA landfilling limits. The SPLP leaching results conformed to the limits implying that the waste or S/S products can be disposed of at a segregated landfill; however the low ANC of the S/S products reveals that there may be leaching in the long-term. The sand used in the mortar samples adversely affected the S/S performance, causing higher heavy metal leaching levels, and lower pH levels in the leachate after the TCLP extraction than those measured in the leachate of the paste samples.

  4. Chemical, physical, structural and morphological characterization of the electric arc furnace dust.

    PubMed

    Machado, Janaína G M S; Brehm, Feliciane Andrade; Moraes, Carlos Alberto Mendes; Santos, Carlos Alberto Dos; Vilela, Antônio Cezar Faria; Cunha, João Batista Marimon da

    2006-08-25

    Electric arc furnace dust (EAFD) is a hazardous industrial waste generated in the collection of particulate material during steelmaking process via electric arc furnace. Important elements to the industry such as, Fe and Zn are the main ones in EAFD. Due to their presence, it becomes very important to know how these elements are combined before studying new technologies for its processing. The aim of this work was to carry out a chemical, physical, structural and morphological characterization of the EAFD. The investigation was carried out by using granulometry analysis, chemical analysis, scanning electron microscopy (SEM), energy dispersive spectroscopy via SEM (EDS), X-ray mapping analysis via SEM, X-ray diffraction (XRD) and Mössbauer spectroscopy. By XRD the following phases were detected: ZnFe(2)O(4), Fe(3)O(4), MgFe(2)O(4), FeCr(2)O (4), Ca(0.15)Fe(2.85)O(4), MgO, Mn(3)O(4), SiO(2) and ZnO. On the other hand, the phases detected by Mössbauer spectroscopy were: ZnFe(2)O(4), Fe(3)O(4), Ca(0.15)Fe(2.85)O(4) and FeCr(2)O(4). Magnesium ferrite (MgFe(2)O(4)), observed in the XRD pattern as overlapped peaks, was not identified in the Mössbauer spectroscopy analysis.

  5. Waste Heat Recovery from High Temperature Off-Gases from Electric Arc Furnace

    SciTech Connect

    Nimbalkar, Sachin U; Thekdi, Arvind; Keiser, James R; Storey, John Morse

    2014-01-01

    This article presents a study and review of available waste heat in high temperature Electric Arc Furnace (EAF) off gases and heat recovery techniques/methods from these gases. It gives details of the quality and quantity of the sensible and chemical waste heat in typical EAF off gases, energy savings potential by recovering part of this heat, a comprehensive review of currently used waste heat recovery methods and potential for use of advanced designs to achieve a much higher level of heat recovery including scrap preheating, steam production and electric power generation. Based on our preliminary analysis, currently, for all electric arc furnaces used in the US steel industry, the energy savings potential is equivalent to approximately 31 trillion Btu per year or 32.7 peta Joules per year (approximately $182 million US dollars/year). This article describes the EAF off-gas enthalpy model developed at Oak Ridge National Laboratory (ORNL) to calculate available and recoverable heat energy for a given stream of exhaust gases coming out of one or multiple EAF furnaces. This Excel based model calculates sensible and chemical enthalpy of the EAF off-gases during tap to tap time accounting for variation in quantity and quality of off gases. The model can be used to estimate energy saved through scrap preheating and other possible uses such as steam generation and electric power generation using off gas waste heat. This article includes a review of the historical development of existing waste heat recovery methods, their operations, and advantages/limitations of these methods. This paper also describes a program to develop and test advanced concepts for scrap preheating, steam production and electricity generation through use of waste heat recovery from the chemical and sensible heat contained in the EAF off gases with addition of minimum amount of dilution or cooling air upstream of pollution control equipment such as bag houses.

  6. Graphite furnace atomic absorption spectrometric determination of lead and cadmium extracted from ceramic foodware: Collaborative Study.

    PubMed

    Hight, S C

    2000-01-01

    A modification of the official flame atomic absorption spectrometric (FAAS) method for determining lead and cadmium extracted from ceramic foodware was collaboratively studied. In the modified method, graphite furnace atomic absorption spectrometry (GFAAS) is substituted for FAAS. The modified method also includes mandatory quality control procedures to improve method performance. The extraction procedure of the official method (leaching with 4% acetic acid for 24 h at room temperature) remains unchanged. Seven laboratories analyzed blind duplicate portions of 3 ceramicware leach solutions containing Pb at concentrations of 0.0196, 0.403, and 3.73 microg/mL and Cd at concentrations of 0.00236, 0.0456, and 0.544 microg/mL. Performance of the modified method compared well with that of the official method. The repeatability relative standard deviation (RSDr) ranged from 0.87 to 6.7% for Pb and from 3.7 to 11% for Cd. The reproducibility relative standard deviation (RSDR) ranged from 4.5 to 12% for Pb and from 7.0 to 11% for Cd. Accuracy of collaborator results was 97-98% for Pb and 93-101% for Cd. Quality control results and quantitation limits were excellent. Method quantitation limits varied among laboratories from 0.005 to 0.019 microg/mL for Pb and from 0.0004 to 0.0019 microg/mL for Cd. The modified method was adopted First Action by AOAC INTERNATIONAL.

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

    PubMed

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

    2016-06-20

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

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

    PubMed

    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.

  9. Stability of low concentration calibration standards for graphite furnace atomic absorption spectrophotometry

    SciTech Connect

    Bass, D A; TenKate, L B

    1993-11-01

    Graphite furnace atomic absorption spectrophotometry (GFAAS) is used for determination of ultra-trace metals in environmentally important samples. In the generation of GFAAS calibration curves for many environmental applications, low concentration calibration standards must be prepared dally, as required by the Statement of Work (SOW) for the US Environmental Protection Agency (EPA) Contract Laboratory Program (CLP). This results in significant time and work for the analyst and significant cost to the Analytical Chemistry Laboratory (ACL) for chemicals and waste management. While EPA SW 846 is less prescriptive than the CLP SOW, ACL has been following the CLP guidelines because in-house criteria regarding the stability of GFAAS standards have not been established. A study was conducted to determine the stability of GFAAS standards for analytes commonly used in the ACL (single and mixed) as a function of time. Data were collected over nine months. The results show that GFAAS standards for Sb, Pb, Se, Ag, and TI are stable for a longer period of time than currently assumed by the CLP SOW. Reducing the frequency of preparing these standards will increase efficiency, decrease the handling of hazardous the quantity of hazardous waste generated, and decrease the quantity of hazardous substances to be ordered and stocked by the laboratory. These benefits will improve GFAAS analysis quality, reduce costs, enhance safety, and lower environmental concerns.

  10. Neutralization of cement-asbestos waste by melting in an arc-resistance furnace.

    PubMed

    Witek, Jerzy; Kusiorowski, Robert

    2017-08-12

    The paper presents the results of research on asbestos waste disposal by the melting process. The tests were carried out in a laboratory arc-resistance electric furnace. The obtained results showed that the fibrous structure of asbestos contained in cement-asbestos waste was completely destroyed. This led to the formation of new mineral phases without dangerous properties. The melting test was conducted on raw cement-asbestos samples without any additives and with a content of mineral compounds, the aim of which was to support the melting process. The additives were selected among others on the basis of the computer simulation results carried out using FactSage database computing system. The research results indicate that the melting process of asbestos wastes is a potential and interesting method of neutralizing hazardous asbestos waste, which allows for further treatment and material recycling. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Reduction Kinetics of Electric Arc Furnace Oxidizing Slag by Al-Fe Alloy

    NASA Astrophysics Data System (ADS)

    Lee, Jaehong; Oh, Joon Seok; Lee, Joonho

    2016-09-01

    Effects of temperature and slag basicity on the reduction rate of iron oxide in molten synthetic electric arc furnace oxidizing slag by Al-40 wt.%Fe alloy was investigated. An alloy sample was dropped into molten slag in an MgO crucible. When the initial slag temperature was 1723 K, there was no reduction. However, when the initial slag temperature was 1773 K and the slag basicity was 1.1, the reduction was initiated and the temperature of the slag rapidly increased. When the slag basicity was 1.1, increasing the initial slag temperature from 1773 K to 1823 K increases the reaction rate. As the slag basicity increased from 1.1 to 1.4 at 1773 K, the reaction rate increased. From SEM analysis, it was found that an Al2O3 or a spinel phase at the slag-metal interface inhibited the reaction at a lower temperature and a lower slag basicity.

  12. The efficiency of quartz addition on electric arc furnace (EAF) carbon steel slag stability.

    PubMed

    Mombelli, D; Mapelli, C; Barella, S; Gruttadauria, A; Le Saout, G; Garcia-Diaz, E

    2014-08-30

    Electric arc furnace slag (EAF) has the potential to be re-utilized as an alternative to stone material, however, only if it remains chemically stable on contact with water. The presence of hydraulic phases such as larnite (2CaO SiO2) could cause dangerous elements to be released into the environment, i.e. Ba, V, Cr. Chemical treatment appears to be the only way to guarantee a completely stable structure, especially for long-term applications. This study presents the efficiency of silica addition during the deslagging period. Microstructural characterization of modified slag was performed by SEM and XRD analysis. Elution tests were performed according to the EN 12457-2 standard, with the addition of silica and without, and the obtained results were compared. These results demonstrate the efficiency of the inertization process: the added silica induces the formation of gehlenite, which, even in caustic environments, does not exhibit hydraulic behaviour.

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

    SciTech Connect

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

    1995-11-01

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

  14. Thermodynamic analysis of the selective carbothermic reduction of electric arc furnace dust.

    PubMed

    Pickles, C A

    2008-01-31

    Electric arc furnace (EAF) dust, which is produced as a result of the melting of automobile scrap in an electric arc furnace, contains considerable amounts of zinc and lead, which are of significant economic value. Typically, the other major components are iron oxide and calcium oxide with minor amounts of other metal oxides. In this research, a detailed thermodynamic study of the pyrometallurgical processing of the dust, using carbon as a reducing agent was performed. The SOLGASMIX solver of Outokumpu HSC Chemistry((R)) 5.1 was used to calculate the equilibrium composition under reducing conditions. The control input dust composition was as follows (in mass percent): 8.100% CaO, 8.250% 2CaO.SiO(2), 11.200% CaCO(3), 8.830% CaO.Fe(2)O(3), 7.840% Fe(3)O(4), 3.770% PbO, 38.150% ZnFe(2)O(4) and 13.860% ZnO. Selective reduction and separation of both the zinc and the lead as metallic vapours, from the iron, in oxide form, was examined. The separation of the zinc or the lead from the iron, was defined quantitatively in terms of the selectivity factor (logbeta) as follows. Equation [see the text] where the subscript symbols refer to the metal being present in gaseous (g), metallic solid (m), solid oxide (o) or metallic liquid (l) form, respectively. The standard calculations were performed for one hundred grams of dust at atmospheric pressure. The variables investigated were as follows; temperature in the range of 1273-1873K, reactant ratio (i.e. moles of carbon per gram of dust), dust composition, addition of inert gas and reduced total pressure. The calculated values were in reasonable agreement with those from previously published studies and also industrial results.

  15. Modeling of zinc solubility in stabilized/solidified electric arc furnace dust.

    PubMed

    Fernández-Olmo, Ignacio; Lasa, Cristina; Irabien, Angel

    2007-06-18

    Equilibrium models which attempt for the influence of pH on the solubility of metals can improve the dynamic leaching models developed to describe the long-term behavior of waste-derived forms. In addition, such models can be used to predict the concentration of metals in equilibrium leaching tests at a given pH. The aim of this work is to model the equilibrium concentration of Zn from untreated and stabilized/solidified (S/S) electric arc furnace dust (EAFD) using experimental data obtained from a pH-dependence leaching test (acid neutralization capacity, ANC). EAFD is a hazardous waste generated in electric arc furnace steel factories; it contains significant amounts of heavy metals such as Zn, Pb, Cr or Cd. EAFD from a local factory was characterized by X-ray fluorescence (XRF), acid digestion and X-ray diffraction (XRD). Zn and Fe were the main components while the XRD analysis revealed that zincite, zinc ferrite and hematite were the main crystalline phases. Different cement/EAFD formulations ranging from 7 to 20% dry weight of cement were prepared and subjected to the ANC leaching test. An amphoteric behavior of Zn was found from the pH dependence test. To model this behavior, the geochemical model Visual MINTEQ (VMINTEQ) was used. In addition to the geochemical model, an empirical model based on the dissolution of Zn in the acidic zone and the re-dissolution of zinc compounds in the alkaline zone was considered showing a similar prediction than that obtained with VMINTEQ. This empirical model seems to be more appropriate when the metal speciation is unknown, or when if known, the theoretical solid phases included in the database of VMINTEQ do not allow to describe the experimental data.

  16. Recycling of an electric arc furnace flue dust to obtain high grade ZnO.

    PubMed

    Ruiz, Oscar; Clemente, Carmen; Alonso, Manuel; Alguacil, Francisco Jose

    2007-03-06

    The production of steel in electric arc furnace (EAF) generates a by-product called EAF dusts. These steelmaking flue dusts are classified in most industrialized countries as hazardous residues because the heavy metals contained in them, tend to leach under slightly acidic rainfall conditions. However, and at the same time they contain zinc species which can be used as a source to obtain valuable by-products. The present investigation shows results on the processing of an EAF flue dust using ammonium carbonate solutions. Once zinc is dissolved: ZnO + 4NH3 + H2O --> Zn(NH3)4(2+) + 2OH- with other impurities (i.e. cadmium and copper), these are eliminated from the zinc solution via cementation with metallic zinc. The purified zinc solution was evaporated (distilled) until precipitation of a zinc carbonate species, which then was calcined to yield a zinc oxide of a high grade. For the unattacked dust residue from the leaching operation, mainly composed of zinc ferrite, several options can be considered: back-recycling to the furnace, further treatment by sodium hydroxide processing or a more safely dumping due to its relatively inertness.

  17. A review of the use of anthracite in electric arc furnace steelmaking

    SciTech Connect

    Rozelle, P.L.

    1994-12-31

    The applications of anthracite in Electric Arc Furnace (EAF) steelmaking, include the adjustment of hot metal carbon content, the generation of foamy slags, and its use as a support fuel in the EAF to reduce power consumption per tonne of product. Incentives to use support fuel in EAF steelmaking include the reduction of electric power consumption without reducing plant output. As such, the concept can reduce steelmaking costs and can serve as a basis for maximizing an EAF operation`s demand side management program. The use of carbon and oxygen additions to the EAF can cause significant release of energy within the furnace. This energy can offset a portion of the electrical energy required by the system for production of steel. Reduced consumption of electricity per tonne of hot metal is the result Electrode consumption and tap to tap times can also be reduced. significant interest in the use of anthracite as EAF support fuel, as well as the other applications of anthracite in EAF steelmaking, have combined to establish the EAF steelmaking trade as a significant market sector for anthracite. This discussion is a review of key anthracite properties and production considerations, and their interplay with the requirements of the EAF process.

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

    NASA Astrophysics Data System (ADS)

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

    2017-03-01

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

  19. Graphite Ablation and Thermal Response Simulation Under Arc-Jet Flow Conditions

    NASA Technical Reports Server (NTRS)

    Chen, Y.-K.; Milos, F. S.; Reda, D. C.; Stewart, D. A.; Venkatapathy, Ethiraj (Technical Monitor)

    2002-01-01

    The Two-dimensional Implicit Thermal Response and Ablation program, TITAN, was developed and integrated with a Navier-Stokes solver, GIANTS, for multidimensional ablation and shape change simulation of thermal protection systems in hypersonic flow environments. The governing equations in both codes are demoralized using the same finite-volume approximation with a general body-fitted coordinate system. Time-dependent solutions are achieved by an implicit time marching technique using Gauess-Siedel line relaxation with alternating sweeps. As the first part of a code validation study, this paper compares TITAN-GIANTS predictions with thermal response and recession data obtained from arc-jet tests recently conducted in the Interaction Heating Facility (IHF) at NASA Ames Research Center. The test models are graphite sphere-cones. Graphite was selected as a test material to minimize the uncertainties from material properties. Recession and thermal response data were obtained from two separate arc-jet test series. The first series was at a heat flux where graphite ablation is mainly due to sublimation, and the second series was at a relatively low heat flux where recession is the result of diffusion-controlled oxidation. Ablation and thermal response solutions for both sets of conditions, as calculated by TITAN-GIANTS, are presented and discussed in detail. Predicted shape change and temperature histories generally agree well with the data obtained from the arc-jet tests.

  20. Investigation of Oxidation-Resistant Coatings on Graphite and Molybdenum in Two Arc-Powered Facilities

    NASA Technical Reports Server (NTRS)

    Peters, Roger W.; Rasnick, Thomas A.

    1961-01-01

    A number of leading-edge specimens of ATJ graphite and 0.5-percent titanium-molybdenum alloy were tested in a 6-inch subsonic low-pressure arc-powered tunnel and a 1,500-kw subsonic arc jet to determine the effectiveness of several refractory coatings in preventing the oxidation of these materials. The results indicate that the siliconized coating for the ATJ graphite and the W-2 and Durak MG coatings for the titanium-molybdenum alloy provide adequate protection at temperatures up to 3,000 F for the durations of the tests in these facilities, approximately 70 seconds in the arc tunnel and approximately 10 minutes in the arc jet. Weight losses (less than one-half of 1 percent) experienced by a few of the coated specimens indicate that tests of longer duration in these environments may prove deleterious and that the stability of these coatings may be depreciated under the low-pressure environmental conditions encountered during reentry.

  1. Release of H and He from TiC, stainless steel and graphite by pulsed electron and furnace heating

    SciTech Connect

    Picraux, S.T.; Wampler, W.R.

    1980-01-01

    The release of implanted D and /sup 3/He from TiC coatings, SS 304 and graphite by pulsed electron beam (e-beam) heating and furnace heating has been investigated. Low fluence implants of D or /sup 3/He and saturation fluence D implants have been studied for 0.5 - 1.5 keV D and 3 keV /sup 3/He. The retained D or /sup 3/He was monitored by ion beam analysis. The 50 ns e-beam pulsing resulted in the release of D in all materials and was compared with release during isochronal annealing in a furnace. A substantial enhancement in the fractional D release was found for D saturated TiC (0.25 D to host atom ratio) compared with low fluence implants. In contrast no enhancement of D release was observed for D saturated graphite and SS 304 compared with low fluence implants. Release of /sup 3/He from TiC was also obtained by e-beam pulsed heating and this release was not affected by the presence of saturation concentrations of D. Comparison to furnace anneals and the calculated time evolution of the temperature profiles suggests a simple model for the D release based on diffusion-limited release in the case of pulsed e-beam treatments and trap-limited release in the case of furnace bulk heating. These processes are closely related to hydrogen recycle in tokamaks and have implications for T inventory control and He ash removal.

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

    NASA Astrophysics Data System (ADS)

    Bencs, László; Laczai, Nikoletta; Ajtony, Zsolt

    2015-07-01

    A combination of former convective-diffusive vapor-transport models is described to extend the calculation scheme for sensitivity (characteristic mass - m0) 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 m0 values were determined with the application of a standard THGA furnace, operating either under stopped, or mini-flow (50 cm3 min- 1) of the internal sheath gas during atomization. The theoretical and experimental ratios of m0(mini-flow)-to-m0(stop-flow) were closely similar for each study analyte. Likewise, the calculated m0 data gave a fairly good agreement with the corresponding experimental m0 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.

  3. Role of a binary metallic modifier in the determination of cadmium in graphite furnace atomic absorption spectrometry.

    PubMed

    Morimoto, Syun; Ashino, Tetsuya; Wagatsuma, Kazuaki

    2010-01-01

    In order to discuss the matrix modifier effect of palladium, iron, and a mixture of palladium and iron for the determination of cadmium in graphite-furnace atomic absorption spectrometry (GF-AAS), we measured the absorption profiles of a cadmium line at various compositions of these elements. Variations in the gas temperature were also estimated with the progress of atomization, by using a two-line method under the assumption of a Boltzmann distribution. The atomic absorption of cadmium appeared on the way of heating from the charring temperature to the atomizing temperature while the gas temperature was still low; it was thus considered that cadmium was atomized through direct conductive heating from the wall of the graphite furnace. Therefore, the effectiveness of modifiers for cadmium would be determined through any reactions on the furnace wall at the programmed charring and atomizing temperatures. The addition of iron, palladium, and an iron-palladium mixture all enhanced the absorption signal of cadmium compared to a pure cadmium sample; however, their effects were different from one another. Each addition of iron or palladium to the sample solution led to an enhancement of the cadmium absorbance, indicating that iron or palladium individually became an effective matrix modifier for the determination of cadmium. However, the addition of palladium was ineffective for the matrix modification in the coexistence of large amounts of iron. Although these phenomena are very complicated, and thus cannot be understood completely, any metallurgical reaction between the constituent elements during heating of the furnace wall, such as the formation of solid solutions and intermetallic compounds, would cause the effect of a matrix modifier in GF-AAS.

  4. [Determination of Pb and Al in blood and hair of child using transverse heated graphite furnace atomic absorption spectroscopy].

    PubMed

    Niu, Feng-lan; Xie, Wen-bing; Li, Chen-xu; Dong, Wei-yan

    2005-04-01

    Pb and Al in blood and hair of child were determined by transverse heated graphite furnace atomic absorption spectrometry with NH4H2PO4 and Mg(NO3)2 as a modifier, which enhanced the temperature of ashing, eliminated the matrix interference and memorial effect. The method is rapid, simple and accurate. The characteristic mass of the method was 2.3 x 10(-11) g and 2.2 x 10(-11) g for Pb and Al respectively. The relative standard deviation of Pb and Al was 3.0% and 11.4%, respectively, and the recovery was 96%-102%.

  5. Spectrometric analysis of non-metals introduced from a graphite furnace into a microwave-induced plasma.

    PubMed

    Matosek, J P; Orr, B J; Selby, M

    1986-11-01

    A low-power helium microwave-induced plasma, sustained in a cylindrical TM(010) cavity, has been used with sample introduction from a graphite furnace. An end-on optical configuration was employed to monitor both atomic and ionic emission from Cl, I, S and P. The operating parameters were optimized with respect to the nature of the plasma background response, the limits of detection, and the shapes and linearity ranges of the log-log analytical working curves. Possible applications were evaluated by determining iodine in milk and analysing a multi-component mixture of sulphur compounds.

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

    PubMed

    Kashefiolasl, Sepide; Foerch, Christian; Pfeilschifter, Waltraud

    2013-02-15

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

  7. The spectral opacity of triatomic carbon measured in a graphite tube furnace over the 280 to 600 nm wavelength range

    NASA Technical Reports Server (NTRS)

    Snow, W. L.; Wells, W. L.

    1980-01-01

    The opacity of linear triatomic carbon (C3) was measured in a graphite tube furnace from 280 to 600 nm to supplement the earlier measurements of Brewer and Engelke. The spectral cross section was estimated from the opacities using temperature profiles determined pyrometrically and a revised heat of formation delta H = 198 kcal/mole). The cross section was found to be nonnegligible over the range 300 to 500 nm and the electronic oscillator strength based on the total cross section estimate was 0.02.

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

    PubMed

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

    2017-03-15

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

  9. Graphite furnace and flame atomic-absorption technique for thermoanalytical investigations.

    PubMed

    Kántor, T; Pungor, E; Sztatisz, J; Bezúr, L

    1979-05-01

    Aerosol particles formed from the vapour of electrothermally heated substances were introduced into an acetylene-air flame for atomization and detection. Thus individual observations could be made on condensed phase processes taking place in the furnace. Curves of absorbance vs. furnace temperature for several zinc compounds were recorded and compared with the corresponding thermoanalytical DTG-curves.

  10. Interaction of graphite and ablative materials with CO2-laser, carbon-arc, and xenon-arc radiation. M.S. Thesis - George Washington Univ., Washington, D. C.

    NASA Technical Reports Server (NTRS)

    Brewer, W. D.

    1975-01-01

    The behavior of graphite and several charring ablators in a variety of high radiative heat flux environments was studied in various radiative environments produced by a CO2 laser and a carbon arc facility. Graphite was also tested in xenon arc radiation. Tests were conducted in air nitrogen, helium, and a mixture of CO2 and nitrogen, simulating the Venus atmosphere. The experimental results are compared with theoretical results obtained with a one dimensional charring ablator analysis and a two dimensional subliming ablator analysis. Photomicroscopy showed no significant differences in appearance or microstructure of the charring ablators or graphite after testing in the three different facilities, indicating that the materials respond fundamentally the same to the radiation of different frequencies. The performance of phenolic nylon and graphite was satisfactorily predicted with existing analyses and published material property data.

  11. Behavior of Zn and Fe Content in Electric Arc Furnace Dust as Submitted to Chlorination Methods

    NASA Astrophysics Data System (ADS)

    Santos, Felipe; Brocchi, Eduardo; Araújo, Victor; Souza, Rodrigo

    2015-08-01

    This work covers initially a general thermodynamics assessment regarding the zinc ferrite (ZnFe2O4) behavior toward direct and reducing chlorination. Then, the use of alternative chlorination agents were also theoretically appreciated, before a set of experiments has been carried out with industrial residue (electric arc furnace dust). Besides identifying zinc ferrite (95.4 pct), the XRD analysis indicated the presence of ZnO (4.6 pct). Therefore, the main objective of the present work is related to a theoretical (thermodynamics) and experimental (kinetics) evaluation of the mentioned residue chemical behavior as submitted to chlorination methods. Several characterization methods were used, such as X-ray diffraction, scanning electron microscopy, X-ray fluorescence, mass spectroscopy (ICP-MS), and energy-dispersive X-ray spectroscopy (EDS). It was observed that zinc was present, mostly, in the form of zinc ferrite (franklinite). The thermodynamics study revealed that Zn has a more susceptible behavior regarding the oxides conversion into chlorides. However, this tendency is not necessarily associated with a selective reaction, as showed for the chlorination in the presence of carbon, as both iron and zinc chlorides formation is feasible. The experimental results have indicated that some reaction systems can be further studied in order to identify operational conditions that enable selective formations. So, it was observed that for the calcium chloride reaction conducted at 1273 K (1000 °C) for 30 minutes, the iron content in the residue slightly increases (with 15 pct removal), whereas the zinc content decreases from 20 to 12 pct (53 pct removal), suggesting complementary studies where this possible selectivity could be even more determinant. Such results have also indicated that the direct action of chlorine at 1073 K (800 °C) allowed complete removal of zinc, followed by conversion in the order of 40 pct in iron. Therefore, a complementary investigation over

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

    NASA Astrophysics Data System (ADS)

    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.

  13. HRTEM analyses of the platinum nanoparticles prepared on graphite particles using coaxial arc plasma deposition

    NASA Astrophysics Data System (ADS)

    Miyazawa, Kun'ichi; Yoshitake, Masaru; Tanaka, Yumi

    2017-06-01

    Platinum nanoparticles with diameters less than ˜5 nm were prepared on graphite particles by the coaxial arc plasma deposition, and the structure of platinum nanoparticles was investigated using high-resolution transmission electron microscopy. {110} facets of platinum nanoparticles parallel to the surface (0001) planes of graphite particles were most frequently observed. The platinum nanoparticles were found to be anisotropically deformed from the bulk face-centered cubic structure, and the lattice parameters of platinum nanoparticles were estimated by assuming monoclinic structures. No correlation was observed between the diameter and the lattice parameters of the platinum nanoparticles. Approximately two-thirds of the platinum nanoparticles were compressively strained, and the other platinum nanoparticles showed the expanded unit cells. The cube root of monoclinic unit cell of the platinum nanoparticles varied from a compression of 5.9% to an expansion of 2.8% as compared with the bulk lattice constant of platinum.

  14. Determination of trace chromium in water by graphite furnace atomic absorption spectrophotometry after preconcentration on a soluble membrane filter

    SciTech Connect

    Gao Piying; Feng Ruolan; Zhang Huaizhu; Li Zhiqiang

    1998-04-01

    A new concentration and determination method has been described for the determination of lower than 0.1 {micro}g L{sup {minus}1} levels of chromium (VI) in water, based on the reaction between chromium (VI) and phenylfluorone (PF) to form an anionic chelate and the collection of the ternary ion-associate of the chelate with cetyltrimethylammonium bromide (CTMAB) (a cationic surfactant) on an organic solvent-soluble membrane filter. Determination of the solution obtained after dissolving the membrane and analyte in a suitable solvent is achieved using graphite furnace atomic absorption spectrophotometry. The ternary complex (Cr(VI)-PF-CTMAB = 1:2:2) is collected on a 0.45 {micro}m nitrocellulose filter and the filter and analyte are dissolved in a small volume of 2-methoxyethanol acidified with dilute sulfuric acid. The chromium is determined by graphite furnace atomic absorption spectrophotometry under optimum experimental conditions. A good linear relationship exists in the range 0.05--0.30 {micro}g chromium in 5.0 ml, with satisfactory reproducibility. The detection limit, defined as three times the standard deviation of the blank, is 0.06 {micro}g L{sup {minus}1} with 20 fold preconcentration. The ions normally present in water do not interfere under the experimental conditions used. The proposed method has been applied to the concentration and determination of chromium (VI) in water samples from several sources by means of direct graphic furnace atomic absorption spectrophotometry; the recoveries of chromium (VI) added to the samples are quantitative, and results found are satisfactory.

  15. Hydrometallurgical process for zinc recovery from electric arc furnace dust (EAFD): part I: Characterization and leaching by diluted sulphuric acid.

    PubMed

    Oustadakis, P; Tsakiridis, P E; Katsiapi, A; Agatzini-Leonardou, S

    2010-07-15

    The present paper is the first of a series of two articles dealing with the development of an integrated process for the recovery of zinc from electric arc furnace dust (EAFD), a hazardous industrial waste generated in the collection of particulate material during steelmaking process via electric arc furnace. Part I presents the EAFD characterization and its leaching process by diluted sulphuric acid, whereas Part II deals with the purification of the leach liquor and the recovery of zinc by solvent extraction/electrowinning. The characterization of the examined electric arc furnace dust was carried out by using granulometry analysis, chemical analysis, X-ray diffraction (XRD), thermogravimetric/differential thermal analysis (TG/DTA) and scanning electron microscopy (SEM). The leaching process was based on the Zn extraction with diluted sulphuric acid from EAFD under atmospheric conditions and without using any preliminary treatment. Statistical design and analysis of experiments were used, in order to determine the main effects and interactions of the leaching process factors, which were: acid normality, temperature and solid to liquid ratio. The zinc recovery efficiency on the basis of EAFD weight reached 80%. X-ray diffraction and scanning electron microscopy were used for the characterization of the leached residues.

  16. Formation of the ZnFe2O4 phase in an electric arc furnace off-gas treatment system.

    PubMed

    Suetens, T; Guo, M; Van Acker, K; Blanpain, B

    2015-04-28

    To better understand the phenomena of ZnFe2O4 spinel formation in electric arc furnace dust, the dust was characterized with particle size analysis, X-ray fluorescence (XRF), electron backscatter diffraction (EBSD), and electron probe micro-analysis (EPMA). Different ZnFe2O4 formation reaction extents were observed for iron oxide particles with different particle sizes. ZnO particles were present as both individual particles and aggregated on the surface of larger particles. Also, the slag particles found in the off-gas were shown not to react with the zinc vapor. After confirming the presence of a ZnFe2O4 formation reaction, the thermodynamic feasibility of in-process separation - a new electric arc furnace dust treatment technology - was reevaluated. The large air intake and the presence of iron oxide particles in the off-gas were included into the thermodynamic calculations. The formation of the stable ZnFe2O4 spinel phase was shown to be thermodynamically favorable in current electric arc furnace off-gas ducts conditions even before reaching the post combustion chamber. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Leaching properties of electric arc furnace dust prior/following alkaline extraction.

    PubMed

    Orescanin, Visnja; Mikelić, Luka; Sofilić, Tahir; Rastovcan-Mioc, Alenka; Uzarević, Krunoslav; Medunić, Gordana; Elez, Loris; Lulić, Stipe

    2007-02-15

    This study was carried out to determine the appropriate treatment of electric arc furnace (EAF) dust prior to permanent disposal. The total heavy metal content as well as heavy metal leaching from EAF dust was investigated in five composite samples obtained from three Croatian and Slovenian steelworks. In order to recover zinc and reduce its leaching from the dust, all five samples were submitted to alkaline extraction with 10 M NaOH. Reduction of Cr (VI) to Cr(III) was conducted using FeSO4 x 7H2O solution. The elements Mn, Fe, Cu, Ni, and notably Zn and Pb, exhibited highest mobility during toxicity characteristic leaching procedure (TCLP). Comparing to TCLP extracts of initial EAF dust, zinc was found to be over 15 times lower and lead over 200 times lower in TCLP extracts of EAF dust processed by the alkaline leaching method. Since Cr (VI) exceeded its permissible level in the DIN 38414-S4 extracts of both initial and alkaline digested dust, its reduction to Cr (III) prior to permanent disposal is necessary. The recovery of zinc from EAF dust treated with alkaline agent ranged from 50.3% to 73.2%. According to phase analysis, recovery yield showed dependence on zincite/franklinite ratio. The results of the study indicate that permanent disposal of EAF dust require the following procedure: alkaline digestion (followed by leachate purification and alkaline zinc electrolyses), chromate reduction (if necessary), solidification of leaching residue and its testing using the leaching analyses.

  18. Electric arc furnace dust as an alternative low-cost oxygen carrier for chemical looping combustion.

    PubMed

    Kuo, Yu-Lin; Huang, Wei-Chen; Tseng, Yao-Hsuan; Chang, Shu-Huai; Ku, Young; Lee, Hao-Yeh

    2017-08-12

    The relative abundance and low cost of electric arc furnace dust (EAFD) make it a viable oxygen carrier for chemical looping combustion (CLC) system. Under a reducing agent, zinc ferrite (ZnFe2O4) phase in EAFD releases zinc vapor in a complex gas-solid reaction. In an effort to suppress the emission of zinc vapor, the reaction mechanism of ZnFe2O4 prepared as an oxygen carrier in a redox cycling test is primarily discussed, as well as the issue of coupling with an inert Al2O3 support. The study focused the investigation on redox cycling behavior and CO2 conversion in ZnFe2O4/Al2O3 and EAFD/Al2O3 systems using a thermogravimetric analyzer (TGA) and fixed-bed reactor (FxBR). In a lab-scaled semi-fluidized bed reactor (semi-FzBR) of EAFD/Al2O3 as an oxygen carrier system, a high CO gas yield approximately 0.98 after fifty redox cycles is also experimentally obtained. It can be anticipated that the use of EAFD/Al2O3 system as an oxygen carrier in a reversible CLC process could be economical and environmentally beneficial. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Review of Innovative Energy Savings Technology for the Electric Arc Furnace

    NASA Astrophysics Data System (ADS)

    Lee, Baek; Sohn, Il

    2014-09-01

    A review of the energy innovations for the electric arc furnace (EAF) steelmaking route is discussed. Preheating of scrap using vertical and horizontal shafts that have been commercially successful in lowering the energy consumption to as much as 90 kWh/t reaching almost the operational limit to heating input scrap materials into the EAF is discussed. Bucket-type and twin-shell preheaters have also shown to be effective in lowering the overall power consumption by 60 kWh/t, but these have been less effective than the vertical shaft-type preheaters. Beyond the scrap preheating technologies, the utilization of waste heat of the slags from the laboratory scale to the pilot scale has shown possible implementation of a granulation and subsequent heat exchange with forced air for energy recovery from the hot slags. Novel techniques to increase metal recovery have shown that laboratory-scale testing of localized Fe concentration into the primary spinel crystals was possible allowing the separation of an Fe-rich crystal from an Fe-depleted amorphous phase. A possible future process for converting the thermal energy of the CO/CO2 off-gases from the EAF into chemical energy was introduced.

  20. Experimental study of the mechanical stabilization of electric arc furnace dust using fluid cement mortars.

    PubMed

    Ledesma, E F; Jiménez, J R; Ayuso, J; Fernández, J M; Brito, J de

    2017-03-15

    This article shows the results of an experimental study carried out in order to determine the maximum amount of electric arc furnace dust (EAFD) that can be incorporated into fluid cement-based mortars to produce mechanically stable monolithic blocks. The leaching performance of all mixes was studied in order to classify them according to the EU Council Decision 2003/33/EC. Two mortars were used as reference and three levels of EAFD incorporation were tested in each of the reference mortars. As the incorporation ratio of EAFD/cement increases, the mechanical strength decreases. This is due to the greater EAFD/cement and water/cement ratios, besides the presence of a double-hydrated hydroxide of Ca and Zn (CaZn2(OH)6·2H2O) instead of the portlandite phase (Ca(OH)2) in the mixes made with EAFD, as well as non-hydrated tricalcium silicate. A mass ratio of 2:1 (EAFD: cement-based mortar) can be added maintaining a stable mechanical strength. The mechanical stabilization process also reduced the leaching of metals, although it was not able to reduce the Pb concentration below the limit for hazardous waste. The high amount of EAFD mechanically stabilized in this experimental study can be useful to reduce the storage volume required in hazardous waste landfills.

  1. Assessment of hexavalent chromium release in Malaysian electric arc furnace steel slag for fertilizer usage

    NASA Astrophysics Data System (ADS)

    Bankole, L. K.; Rezan, S. A.; Sharif, N. M.

    2014-03-01

    This study investigates the leaching of hexavalent chromium (Cr (VI)) from electric arc furnace steel slag as Cr (VI) is classified as human carcinogen. Batch leaching tests were performed for 16 days. The lixiviants used were alkaline, de-ionized and rain water. After 16 days, Cr (VI) was found to be highest in alkaline water (0.03 mg/L) and lowest in de-ionized water (0.01 mg/L). Besides the lixiviants used, slag stirring speed and liquid to solid ratio also affect Cr (VI) released. The experimental work was complimented with slag characterization using XRF, XRD and SEM/EDX analysis. The leaching process was also simulated via Factsage software to calculate isothermal pourbaix diagrams. The Cr (VI) released was low and below the threshold of 0.1 mg/L set for public water systems. Recycle the slag as fertilizer should be considered safe as it does not exceed the safety limit set for Cr (VI) dissolution.

  2. Environmental impacts of asphalt mixes with electric arc furnace steel slag.

    PubMed

    Milačič, Radmila; Zuliani, Tea; Oblak, Tina; Mladenovič, Ana; Ančar, Janez Šč

    2011-01-01

    Electric arc furnace (EAF) steel slag can be used as an alternative high-quality material in road construction. Although asphalts with slag aggregates have been recognized as environmentally acceptable, there is a lack of data concerning the potential leaching of toxic Cr(VI) due to the highly alkaline media of EAF slag. Leaching of selected water extractable metals from slag indicated elevated concentrations of total chromium and Cr(VI). To estimate the environmental impacts of asphalt mixes with slag, leachability tests based on diffusion were performed using pure water and salt water as leaching agents. Compact and ground asphalt composites with natural aggregates, and asphalt composites in which the natural aggregates were completely replaced by slag were prepared. The concentrations of total chromium and Cr(VI) were determined in leachates over a time period of 6 mo. After 1 and 6 mo, the concentrations of some other metals were also determined in the leachates. The results indicated that chromium in leachates from asphalt composites with the addition of slag was present almost solely in its hexavalent form. However, the concentrations were very low (below 25 μg L) and did not represent an environmental burden. The leaching of other metals from asphalt composites with the addition of slag was negligible. Therefore, the investigated EAF slag can be considered as environmentally safe substitute for natural aggregates in asphalt mixes. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  3. Integrated hydrometallurgical process for production of zinc from electric arc furnace dust in alkaline medium.

    PubMed

    Youcai, Z; Stanforth, R

    2000-12-30

    In this study, a novel and integrated hydrometallurgical process for the production of zinc powder from electric arc furnace (EAF) dust in alkaline medium is reported. The dust is firstly hydrolysed in water, and then fused in caustic soda at 350 degrees C for 1h, followed by leaching in alkaline solution in which both zinc and lead are effectively extracted. Zinc powder is then produced by electrowinning from the leach solution after the lead is selectively removed by precipitation using sodium sulphide as precipitant. The EAF dust tested contained 25% Zn, 1.8% Pb and 33% Fe. It was found that 38% of zinc and 68% of lead could be extracted from the dust when leached directly in caustic soda solution. Leaching of zinc increased to 80% when dust was directly fused with caustic soda followed by alkaline leaching. However, the leaching further increased to 95% when the dust was hydrolysed first with water before fusion. Zinc powder with a purity of 99.95% was then produced by electrowinning from the lead depleted solution. Stainless electrodes were used as both anode and cathode.

  4. Model of phosphorus precipitation and crystal formation in electric arc furnace steel slag filters.

    PubMed

    Claveau-Mallet, Dominique; Wallace, Scott; Comeau, Yves

    2012-02-07

    The objective of this study was to develop a phosphorus retention mechanisms model based on precipitation and crystallization in electric arc furnace slag filters. Three slag columns were fed during 30 to 630 days with a reconstituted mining effluent at different void hydraulic retention times. Precipitates formed in columns were characterized by X-ray diffraction and transmission electronic microscopy. The proposed model is expressed in the following steps: (1) the rate limiting dissolution of slag is represented by the dissolution of CaO, (2) a high pH in the slag filter results in phosphorus precipitation and crystal growth, (3) crystal retention takes place by filtration, settling and growth densification, (4) the decrease in available reaction volume is caused by crystal and other particulate matter accumulation (and decrease in available reaction time), and (5) the pH decreases in the filter over time if the reaction time is too low (which results in a reduced removal efficiency). Crystal organization in a slag filter determines its phosphorus retention capacity. Supersaturation and water velocity affect crystal organization. A compact crystal organization enhances the phosphorus retention capacity of the filter. A new approach to define filter performance is proposed: saturation retention capacity is expressed in units of mg P/mL voids.

  5. Characterization and leachability of electric arc furnace dust made from remelting of stainless steel.

    PubMed

    Laforest, Guylaine; Duchesne, Josée

    2006-07-31

    Electric arc furnace dust (EAFD) is a toxic waste product made in the remelting of scrap steel. The results of a Toxicity Characteristic Leaching Procedure (TCLP) conducted on a sample of EAFD originating from the remelting of stainless steel scrap showed that the total Cr and Cr (VI) liquor concentrations (9.7 and 6.1 mg/L, respectively) exceeded the Toxicity Characteristic Regulatory Level (TCRL). The EAFD showed a complex heterogeneous mineralogy with spinel minerals group predominance. A sequential extractions method has permitted the determination of the amount of available metals (potentially mobile component) from the EAFD as follows: Cr (3%), Ni (6%), Pb (49%) and Zn (40%). Solubility controls on Cr, Pb, Zn and Ni were identified in the EAFD. This means that the Cr, Pb, Zn and Ni concentrations in solution were controlled by the solubility of some phases from EAFD. The concentrations of Ni and Zn, which are metals not regulated by TCRL were below 0.41 and 1.3 mg/L, respectively. The solubility control on Pb was sufficient to decrease its concentration (<0.24 mg/L) to a level below the TCRL. However, the control on Cr was not sufficient to decrease its concentration (between 117 and 331 mg/L) to below the TCRL.

  6. Valorisation of electric arc furnace steel slag as raw material for low energy belite cements.

    PubMed

    Iacobescu, R I; Koumpouri, D; Pontikes, Y; Saban, R; Angelopoulos, G N

    2011-11-30

    In this paper, the valorisation of electric arc furnace steel slag (EAFS) in the production of low energy belite cements is studied. Three types of clinkers were prepared with 0 wt.% (BC), 5 wt.% (BC5) and 10 wt.% (BC10) EAFS, respectively. The design of the raw mixes was based on the compositional indices lime saturation factor (LSF), alumina ratio (AR) and silica ratio (SR). The clinkering temperature was studied for the range 1280-1400°C; firing was performed at 1380°C based on the results regarding free lime and the evolution of microstructure. In order to activate the belite, clinkers were cooled fast by blown air and concurrent crushing. The results demonstrate that the microstructure of the produced clinkers is dominated by belite and alite crystals, with tricalcium aluminate and tetracalcium-alumino-ferrite present as micro-crystalline interstitial phases. The prepared cements presented low early strength development as expected for belite-rich compositions; however the 28-day results were 47.5 MPa, 46.6 MPa and 42.8 MPa for BC, BC5 and BC10, respectively. These values are comparable with OPC CEMI 32.5 N (32.5-52.5 MPa) according to EN 197-1. A fast setting behaviour was also observed, particularly in the case of BC10, whereas soundness did not exceed 1mm.

  7. Steel foundry electric arc furnace dust management: stabilization by using lime and Portland cement.

    PubMed

    Salihoglu, Guray; Pinarli, Vedat

    2008-05-30

    The purpose of this study was to determine an appropriate treatment for steel foundry electric arc furnace dust (EAFD) prior to permanent disposal. Lime and Portland cement (PC)-based stabilization was applied to treat the EAFD that contains lead and zinc above the landfilling limits, and is listed by USEPA as hazardous waste designation K061 and by EU as 10 02 07. Three types of paste samples were prepared with EAFD content varying between 0 and 90%. The first type contained the EAFD and Portland cement, the second contained the EAFD, Portland cement, and lime, and the third contained the EAFD and lime. All the samples were subjected to toxicity characteristics leaching procedure (TCLP) after an air-curing period of 28 days. pH changes were monitored and acid neutralization capacity of the samples were examined. Treatment effectiveness was evaluated in terms of reducing the heavy metal leachability to the levels below the USEPA landfilling criteria. An optimum composition for the EAFD stabilization was formulated as 30% EAFD +35% lime +35% Portland cement to achieve the landfilling criteria. The pH interval, where the solubility of the heavy metals in the EAFD was minimized, was found to be between 8.2 and 9.4.

  8. Achieving zero waste of municipal incinerator fly ash by melting in electric arc furnaces while steelmaking.

    PubMed

    Yang, Gordon C C; Chuang, Tsun-Nan; Huang, Chien-Wen

    2017-02-25

    The main objective of this work was to promote zero waste of municipal incinerator fly ash (MIFA) by full-scale melting in electric arc furnaces (EAFs) of steel mini mills around the world. MIFA, generally, is considered as a hazardous waste. Like in many countries, MIFA in Taiwan is first solidified/stabilized and then landfilled. Due to the scarcity of landfill space, the cost of landfilling increases markedly year by year in Taiwan. This paper presents satisfactory results of treating several hundred tons of MIFA in a full-scale steel mini mill using the approach of "melting MIFA while EAF steelmaking", which is somewhat similar to "molten salt oxidation" process. It was found that this practice yielded many advantages such as (1) about 18wt% of quicklime requirement in EAF steelmaking can be substituted by the lime materials contained in MIFA; (2) MIFA would totally end up as a material in fractions of recyclable EAF dust, oxidized slag and reduced slag; (3) no waste is needed for landfilling; and (4) a capital cost saving through the employment of existing EAFs in steel mini mills instead of building new melting plants for the treatment of MIFA. Thus, it is technically feasible to achieve zero waste of MIFA by the practice of this innovative melting technology.

  9. Recovery of Zn from acid mine water and electric arc furnace dust in an integrated process.

    PubMed

    Carranza, Francisco; Romero, Rafael; Mazuelos, Alfonso; Iglesias, Nieves

    2016-01-01

    In this paper, the purification of acid mine water and the treatment of electric arc furnace dust (EAFD) are integrated into one process with the aim of recovering the Zn content of both effluent and waste. Zinc recovery can reduce the cost of their environmental management: purified acid mine water is discharged after removing all metals; EAFD ceases to be hazardous waste; and Zn is valorised. The process consists of the recovery of Zn as zinc oxide and its purification into commercial products. First, EAFD is leached with acid water and the dissolved metals are selectively precipitated as hydroxides. After EADF leaching, ferrous iron is bio-oxidized and Fe and Al are then precipitated; in the following stage, Cu, Ni, Co and Cd are cemented and finally Zn is precipitated as ZnO. In order to purify water that finally is discharged to a river, lime is used as the neutralizing agent, which results in a precipitate of mainly gypsum, MnO, and ZnO. From the impure zinc oxide produced, various alternatives for the attainment of commercial products, such as basic zinc carbonate and electrolytic zinc, are studied in this work. Copyright © 2015 Elsevier Ltd. All rights reserved.

  10. Microwave treatment of electric arc furnace dust with PVC: dielectric characterization and pyrolysis-leaching.

    PubMed

    Al-Harahsheh, Mohammad; Kingman, Sam; Al-Makhadmah, Leema; Hamilton, Ian E

    2014-06-15

    Microwave treatment of electric arc furnace dust (EAFD) with poly(vinyl chloride) (PVC) was studied in this work. A comprehensive characterization of the dust as well as assessing the suitability of using the thermal de-chlorination of the common plastic (PVC) under inert atmosphere was carried out to assess the possibility of Zn and other heavy metals extraction (Pb and Cd) from EAFD. The dielectric and thermal properties of EAFD, PVC and their mixtures were measured. Once combined and heated the metal oxides present in the dust reacted with HCl released from PVC during thermal de-chlorination, forming metal chlorides which were subsequently recovered by leaching with water. It was found that zinc chloride could be almost completely recovered in the leaching stage, with the overall recovery of Zn reaching 97% when the EAFD:PVC ratio was 1:2. The investigation highlighted that franklinite, the most refractory mineral to leaching, was completely destroyed. The leaching residue was found to compose mainly of magnetite and hematite. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Recycling of electric arc furnace dust through dissolution in deep eutectic ionic liquids and electrowinning.

    PubMed

    Bakkar, Ashraf

    2014-09-15

    The dust waste formed during steelmaking in electric arc furnace (EAF) is rich in ferrous and nonferrous metals. Recycling of this dust as a raw material in iron or steel-making is hazardous and therefore it is mostly dumped. This paper demonstrates recycling of EAF dust through selective dissolution of metal oxides in a deep eutectic ionic liquid. It was found that about 60% of Zn and 39% of Pb could be dissolved from the dust when stirred for 48h in 1 choline chloride:2 urea ionic liquid at 60°C. The resultant electrolyte was subsequently fed to a conventional three-electrode cell where cyclic voltammetry (CV) measurements were conducted to describe its electrochemical behavior. Two deposition peaks were determined and ascribed to deposition of zinc and lead. Static potentials were successively applied to electrowin metallic zinc. SEM/EDX investigations showed that the zinc electrowon contained remarkable contents of lead. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Method and Mechanisms of Soil Stabilization Using Electric Arc Furnace Dust

    NASA Astrophysics Data System (ADS)

    Al-Amoudi, Omar S. Baghabra; Al-Homidy, Abdullah A.; Maslehuddin, Mohammed; Saleh, Tawfik A.

    2017-04-01

    This paper reports the method and mechanism for improving the strength of marl and desert sand utilizing electric arc furnace dust (EAFD), an industrial by-product, in lieu of cement or lime. EAFD was used in conjunction with a small quantity (2%) of cement. The mechanical properties and durability characteristics of marl and sand mixed with 2% cement plus 5-, 10-, 20- or 30%-EAFD, by weight of the soil, were evaluated. The soil-cement-EAFD mixtures were used to determine their unconfined compressive strength (UCS), soaked California Bearing Ratio (CBR) and durability. The risk of leaching of toxic heavy metals, such as lead and cadmium, from the stabilized soils to the groundwater was also investigated. The mechanisms of stabilization of the selected soils due to the use of EAFD along with a small quantity of cement are also elucidated. The usage of 20 to 30% EAFD with 2% cement was noted to considerably improve the mechanical properties and durability of both marl and sand.

  13. Method and Mechanisms of Soil Stabilization Using Electric Arc Furnace Dust

    PubMed Central

    Al-Amoudi, Omar S. Baghabra; Al-Homidy, Abdullah A.; Maslehuddin, Mohammed; Saleh, Tawfik A.

    2017-01-01

    This paper reports the method and mechanism for improving the strength of marl and desert sand utilizing electric arc furnace dust (EAFD), an industrial by-product, in lieu of cement or lime. EAFD was used in conjunction with a small quantity (2%) of cement. The mechanical properties and durability characteristics of marl and sand mixed with 2% cement plus 5-, 10-, 20- or 30%-EAFD, by weight of the soil, were evaluated. The soil-cement-EAFD mixtures were used to determine their unconfined compressive strength (UCS), soaked California Bearing Ratio (CBR) and durability. The risk of leaching of toxic heavy metals, such as lead and cadmium, from the stabilized soils to the groundwater was also investigated. The mechanisms of stabilization of the selected soils due to the use of EAFD along with a small quantity of cement are also elucidated. The usage of 20 to 30% EAFD with 2% cement was noted to considerably improve the mechanical properties and durability of both marl and sand. PMID:28452346

  14. Computational Fluid Dynamics Modeling of Supersonic Coherent Jets for Electric Arc Furnace Steelmaking Process

    NASA Astrophysics Data System (ADS)

    Alam, Morshed; Naser, Jamal; Brooks, Geoffrey; Fontana, Andrea

    2010-12-01

    Supersonic coherent gas jets are now used widely in electric arc furnace steelmaking and many other industrial applications to increase the gas-liquid mixing, reaction rates, and energy efficiency of the process. However, there has been limited research on the basic physics of supersonic coherent jets. In the present study, computational fluid dynamics (CFD) simulation of the supersonic jet with and without a shrouding flame at room ambient temperature was carried out and validated against experimental data. The numerical results show that the potential core length of the supersonic oxygen and nitrogen jet with shrouding flame is more than four times and three times longer, respectively, than that without flame shrouding, which is in good agreement with the experimental data. The spreading rate of the supersonic jet decreased dramatically with the use of the shrouding flame compared with a conventional supersonic jet. The present CFD model was used to investigate the characteristics of the supersonic coherent oxygen jet at steelmaking conditions of around 1700 K (1427 °C). The potential core length of the supersonic coherent oxygen jet at steelmaking conditions was 1.4 times longer than that at room ambient temperature.

  15. Turning waste into valuable resource: potential of electric arc furnace dust as photocatalytic material.

    PubMed

    Sapiña, M; Jimenez-Relinque, E; Castellote, M

    2014-10-01

    This paper explores the potential of a hazardous waste of difficult management, electric arc furnace dust (EAFD), as photocatalytic material. Starting from a real waste coming from a Spanish steel factory, chemical, mineralogical, and optical characterizations have been carried out. Direct trials on EAFD and mortar containing this waste have been performed to evaluate its potential as photocatalyst itself and within a cementitious material. The analysis of photocatalytic properties has been done by two different methods: degradation of NO x and degradation of rhodamine (RhB). As a result, it can be said that EAFD exhibited photocatalytic activity for both configurations with UV and visible light, having the mortar enhanced photocatalytic activity for NO x with respect to the EAFD itself. Additionally, in direct trials on the EAFD, it has been able to degrade RhB even in the dark, which has been attributed to transfer of electrons between the adsorbed RhB and the conduction band of some oxides in the dust.

  16. Optical Sensors for Post Combustion Control in Electric Arc Furnace Steelmaking (TRP 9851)

    SciTech Connect

    Sarah W. Allendorf; David K. Ottesen; Robert W. Green; Donald R. Hardesty; Robert Kolarik; Howard Goodfellow; Euan Evenson; Marshall Khan; Ovidiu Negru; Michel Bonin; Soren Jensen

    2003-12-31

    Working in collaboration with Stantec Global Technologies, Process Metrix Corporation, and The Timken Company, Sandia National Laboratories constructed and evaluated a novel, laser-based off-gas sensor at the electric arc furnace facility of Timken's Faircrest Steel Plant (Canton, Ohio). The sensor is based on a mid-infrared tunable diode laser (TDL), and measures the concentration and temperature of specific gas species present in the off-gas emanating from the EAF. The laser beam is transmitted through the gas stream at the fourth hole of the EAF, and provides a real-time, in situ measurement that can be used for process optimization. Two sets of field tests were performed in parallel with Stantec's extractive probe off-gas system, and the tests confirm the TDL sensor's operation and applicability for electric steel making. The sensor measures real-time, in situ line-of-sight carbon monoxide (CO) concentrations between 5% and 35% CO, and measures off-gas temperature in the range of 1400 to 1900 K. In order to achieve commercial-ready status, future work is required to extend the sensor for simultaneous CO and CO{sub 2} concentration measurements. In addition, long-term endurance tests including process optimization must be completed.

  17. Effect of electric arc furnace slag on growth and physiology of maize (Zea mays L.).

    PubMed

    Radić, Sandra; Crnojević, Helena; Sandev, Dubravka; Jelić, Sonja; Sedlar, Zorana; Glavaš, Katarina; Pevalek-Kozlina, Branka

    2013-12-01

    Basic slag, used in this study as a potential source of certain nutrients, is a byproduct of the production of steel in electric arc furnace (EAF). A pot experiment with two nutrient-poor substrates was conducted to investigate to compare the effect of EAF steel slag and fertilizers NPK + F e on growth and availability of specific nutrients to maize. Mineral content of both substrate and plant leaves, growth, chlorophyll fluorescence and photosynthetic pigments were measured following six weeks of cultivation. As steel slag also contains trace amounts of heavy metals, certain oxidative parameters (antioxidative enzyme activities and lipid peroxidation) were evaluated as well. The steel slag improved soil mineral composition, increased above ground maize biomass by providing Fe, Mn, Mg, K and partly P and improved photosynthetic parameters. The potential phytotoxicity of EAF slag containing substrates was not determined as evaluated by MDA (malondialdehyde), GR (glutathione reductase) and APX (ascorbate peroxidase) levels. The obtained results show that EAF steel slag is comparable to NPK + F e in supplying nutrients for maize growth, indicating the potential of EAF steel slag as an inexpensive and non-phytotoxic nutrient supplier especially in poor soils.

  18. Analysis of uranium-bearing Fe-phosphide from a submerged arc furnace for phosphorus production

    NASA Astrophysics Data System (ADS)

    Voncken, J. H. L.; Scheepers, E.; Yang, Y.

    2006-10-01

    During a study on the Fe-phosphide phase formed during phosphorus production in a submerged arc furnace, a sample of ferrophosphorus was found which contains a so far unknown uranium-bearing Fe-phosphide. Uranium, as well as other trace metals like Mn, V, Cr, Ni, Zr, originates from the apatite ore used. Ti originates partly from the silica and coke used in the reduction process, but mainly from the clay used to produce ore pellets. In this paper the ferrophosphorus is described with respect to composition and crystalline compounds present. The crystallization sequence is discussed with respect to the FeP-phase diagram. The main phases found in the ferrophosphorus are FeP and Fe2P. With respect to trace and minor metals, it is observed that Si preferably enters the FeP-phase, whereas Ti, V, Cr, Mn and Ni preferably enter the Fe2P-phase, which is an analogue of the mineral barringerite. This study gives some insight into the behavior of impurities during crystallization of an iron-rich Fe-phosphide melt. The uranium-bearing phase has an overall Me2P-stoichiometry (Fe1.59, Ti0.06, V0.03, Cr0.02, Mn0.06, Ni0.02, U0.15, Zr0.09)2.02 (P0.96, Si0.02)0.98. An X-ray diffraction pattern of this phase is given for identification purposes.

  19. Nitrogen Control in Electric Arc Furnace Steelmaking by DRI (TRP 0009)

    SciTech Connect

    Dr. Gordon A. Irons

    2004-03-31

    Nitrogen is difficult to remove in electric arc furnace (EAF) steelmaking, requiring the use of more energy in the oxygen steelmaking route to produce low-nitrogen steel. The objective of this work was to determine if the injection of directly reduced iron (DRI) fines into EAFs could reduce the nitrogen content by creating fine carbon monoxide bubbles that rinse nitrogen from the steel. The proposed work included physical and chemical characterization of DRI fines, pilot-scale injection into steel, and mathematical modeling to aid in scale-up of the process. Unfortunately, the pilot-scale injections were unsuccessful, but some full-scale data was obtained. Therefore, the original objectives were met, and presented in the form of recommendations to EAF steelmakers regarding: (1) The best composition and size of DRI fines to use; (2) The amount of DRI fines required to achieve a specific reduction in nitrogen content in the steel; and (3) The injection conditions. This information may be used by steelmakers in techno-economic assessments of the cost of reducing nitrogen with this technology.

  20. Thermodynamic analysis of the selective chlorination of electric arc furnace dust.

    PubMed

    Pickles, C A

    2009-07-30

    The remelting of automobile scrap in an electric arc furnace (EAF) results in the production of a dust, which contains high concentrations of the oxides of zinc, iron, calcium and other metals. Typically, the lead and zinc are of commercial value, while the other metals are not worth recovering. At the present time, EAF dusts are treated in high temperature Waelz rotary kiln-type processes, where the lead and zinc oxides are selectively reduced and simultaneously reoxidized and a crude zinc oxide is produced. Another alternative processing route is selective chlorination, in which the non-ferrous metals are preferentially chlorinated to their gaseous chlorides and in this manner separated from the iron. In the present research, a detailed thermodynamic analysis of this chlorination process has been performed and the following factors were investigated; temperature, amount of chlorine, lime content, silica content, presence of an inert gas and the oxygen potential. High lead and zinc recoveries as gaseous chlorides could be achieved but some of the iron oxide was also chlorinated. Additionally, the calcium oxide in the dust consumes chlorine, but this can be minimized by adding silica, which results in the formation of stable calcium silicates. The optimum conditions were determined for a typical dust composition. The selectivities achieved with chlorination were lower than those for reduction, as reported in the literature, but there are other advantages such as the potential recovery of copper.

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

    PubMed

    Dobrowolski, Ryszard; Adamczyk, Agnieszka; Otto, Magdalena

    2013-09-15

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

  2. Refractory graphite skimmers for supersonic free-jet, supersonic arc-jet, and plasma discharge applications

    NASA Astrophysics Data System (ADS)

    Jordan, D. C.; Barling, R.; Doak, R. B.

    1999-03-01

    The fabrication of molecular beam "skimmers" from electrical discharge machining (EDM) graphite is reported. EDM graphite is highly refractory and is easily machined using conventional cutting and grinding techniques. In its most fine-grained form, EDM graphite can be machined free-standing to a knife-edge lip radius of ˜1 μm, providing excellent skimmer aerodynamics. Being refractory, such EDM skimmers are of particular interest in sampling or collimating high-temperature plasma discharges. Our explicit application is in skimming an electrical discharge supersonic free-jet of molecular nitrogen, forming a molecular beam of A 3Σu+ metastable N2 to be used in the heteroepitaxial growth of III-N wide-band-gap semiconductors. In view of the their economy, ease of manufacture, and excellent aerodynamics, the skimmers may also find use in skimming conventional, nondischarge supersonic free-jets. The performance of the EDM skimmers was tested in a conventional helium supersonic free-jet expansion, measuring the time-of-flight distribution and beam intensity as a function of nozzle pressure and nozzle-skimmer separation. Direct comparison with commercial nickel and copper skimmers showed the EDM graphite skimmers to perform nearly as well as the best commercial metal skimmers. The refractory properties of the skimmers were tested in a high-temperature arc-discharge supersonic free-jet expansion of 10% nitrogen in argon. Exposure to a plasma plume of ˜7500 K for over 6 h produced only relatively minor deterioration of the EDM graphite skimmer.

  3. Determination of erbium and neodymium dopants in bismuth tellurite optical crystals by graphite furnace atomic spectrometry techniques

    NASA Astrophysics Data System (ADS)

    Bencs, László; Szakács, Ottó; Kántor, Tibor

    1999-08-01

    Application of concentrated HCl as a solvent and triammonium citrate (TAC) as a chemical modifier is advantageous for the determination of Er and Nd dopants in bismuth tellurite (Bi2TeO5) single crystals by graphite furnace atomic absorption spectrometry (GFAAS). The use of mini-flow of the internal gas, instead of gas stop, results in better precision at a price of a relatively small decrease in sensitivity. By evaluating integrated absorbance (Aint) signals for the GFAAS measurements (in the presence of matrix and TAC additive), characteristic mass values of 42 and 320 pg, and a limit of detection (LOD) of 4.9 and 131 μg l-1 are found for Er and Nd, respectively. These LOD data correspond to 0.78 μg g-1 Er and 21 μg g-1 Nd in the solid samples. The calibration curves are linear up to 0.33 and 2.9 mg l-1 concentrations in the solutions of Er and Nd, respectively. The ratio of the Aint signals of Er and Nd under gas stop and mini-flow were found near constant (1.34) with and without the matrix plus TAC. According to the vaporisation studies by graphite furnace electrothermal vaporisation inductively coupled plasma atomic emission spectrometry (GF-ETV-ICP-AES), the vaporisation of Bi and Te components of the solid Bi2TeO5 can be completed at 1200°C in a relatively short time, ensuring a preconcentration for the Er and Nd dopants, which do not vaporise below 2200°C in an argon atmosphere. On the other hand, fast vaporisation can be performed for the analytes at 2200°C with the use of CCl4 vapour (∼0.5 v/v%) in the internal furnace gas (Ar). It was estimated for the Er analyte that by applying 10 mg of solid sample in the GF-ETV device (dispensed into a graphite sample boat) and using a two-step heating procedure (prevaporisation of the matrix in argon and vaporisation of the analyte in a chlorinating atmosphere), the lower limit of the quantitative determination with the ICP-AES method would be approximately one order of magnitude better than attainable with

  4. Determination of Pb in Biological Samples by Graphite Furnace Atomic Absorption Spectrophotometry: An Exercise in Common Interferences and Fundamental Practices in Trace Element Determination

    ERIC Educational Resources Information Center

    Spudich, Thomas M.; Herrmann, Jennifer K.; Fietkau, Ronald; Edwards, Grant A.

    2004-01-01

    An experiment is conducted to ascertain trace-level Pb in samples of bovine liver or muscle by applying graphite furnace atomic absorption spectrophotometry (GFAAS). The primary objective is to display the effects of physical and spectral intrusions in determining trace elements, and project the usual methods employed to minimize accuracy errors…

  5. Determination of Pb in Biological Samples by Graphite Furnace Atomic Absorption Spectrophotometry: An Exercise in Common Interferences and Fundamental Practices in Trace Element Determination

    ERIC Educational Resources Information Center

    Spudich, Thomas M.; Herrmann, Jennifer K.; Fietkau, Ronald; Edwards, Grant A.

    2004-01-01

    An experiment is conducted to ascertain trace-level Pb in samples of bovine liver or muscle by applying graphite furnace atomic absorption spectrophotometry (GFAAS). The primary objective is to display the effects of physical and spectral intrusions in determining trace elements, and project the usual methods employed to minimize accuracy errors…

  6. Determination of bismuth in environmental samples by slurry sampling graphite furnace atomic absorption spectrometry using combined chemical modifiers.

    PubMed

    Dobrowolski, Ryszard; Dobrzyńska, Joanna; Gawrońska, Barbara

    2015-01-01

    Slurry sampling graphite furnace atomic absorption spectrometry technique was applied for the determination of Bi in environmental samples. The study focused on the effect of Zr, Ti, Nb and W carbides, as permanent modifiers, on the Bi signal. Because of its highest thermal and chemical stability and ability to substantially increase Bi signal, NbC was chosen as the most effective modifier. The temperature programme applied for Bi determination was optimized based on the pyrolysis and atomization curves obtained for slurries prepared from certified reference materials (CRMs) of the soil and sediments. To overcome interferences caused by sulfur compounds, Ba(NO₃)₂ was used as a chemical modifier. Calibration was performed using the aqueous standard solutions. The analysis of the CRMs confirmed the reliability of the proposed analytical method. The characteristic mass for Bi was determined to be 16 pg with the detection limit of 50 ng/g for the optimized procedure at the 5% (w/v) slurry concentration.

  7. Determination of cadmium in spring water by graphite-furnace atomic absorption spectrometry after coprecipitation with ytterbium hydroxide.

    PubMed

    Atsumi, Kousuke; Minami, Tomoharu; Ueda, Joichi

    2005-06-01

    A coprecipitation method with ytterbium hydroxide was studied for the determination of cadmium in water samples by graphite-furnace atomic absorption spectrometry. Up to 40 ng of cadmium in water samples was quantitatively coprecipitated with ytterbium hydroxide at pH 8.0-11.2. The concentration factor was 100 fold. The coprecipitated cadmium was sensitively determined without any influence of ytterbium and the calibration curve was linear from 0.1 to 4 ng/mL of cadmium. The detection limit (signal/noise = 2) was 2.9 pg/mL in 100 mL of the initial sample solution. Twenty-nine diverse ions tested did not interfere with the determination in at least a 10000-fold mass ratio to cadmium. The proposed method was successfully applied to the determination of cadmium in spring water.

  8. Electric arc furnaces for steel-making: hot spots for persistent organic pollutants.

    PubMed

    Odabasi, Mustafa; Bayram, Abdurrahman; Elbir, Tolga; Seyfioglu, Remzi; Dumanoglu, Yetkin; Bozlaker, Ayse; Demircioglu, Hulusi; Altiok, Hasan; Yatkin, Sinan; Cetin, Banu

    2009-07-15

    Persistent organic pollutant (POP) concentrations were measured in stack-gases of ferrous scrap processing steel plants with electric arc furnaces (EAFs) (n = 5) in Aliaga, Izmir, Turkey and in air (n = 11) at a site near those plants. Measured stack-gas concentrations for the four plants without scrap preheating (611 +/- 311, 165,000 +/- 285,000, and 33 +/- 3 ng m(-3), average +/- SD for sigma41PCBs, sigma16PAHs, and sigma7PBDEs, respectively) indicated that they are significant sources for polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and polybrominated diphenyl ethers (PBDEs). POP emissions from the plant with scrap preheating were significantly higher (13 500, 445 000, and 91 ng m(-3) for sigma41PCBs, sigma16PAHs, and sigma7PBDEs, respectively). It was also shown that the steel plants emit considerable amounts of fugitive POPs in particle-phase. Estimated emissions using the emission factors generated in this study and the production amounts suggested that the steel plants with EAFs may significantly contribute to local and global PAH, PCB, and PBDE emissions. Several other compounds (aromatic and aliphatic hydrocarbons, oxygen, sulfur, nitrogen, and chlorine-containing organic compounds, n = 49) were identified and determined semiquantitatively in the stack-gas and ambient air samples. Ambient air concentrations (62 +/- 35, 320 +/- 134 ng m(-3), 1451 +/- 954 pg m(-3), for sigma41PCBs, sigma16PAHs, and sigma7PBDEs, respectively) were significantly higher than those measured previously around the world and in the region, further confirming that the steel plants with EAFs are "hot spots" for POPs.

  9. Preliminary Results from Electric Arc Furnace Off-Gas Enthalpy Modeling

    SciTech Connect

    Nimbalkar, Sachin U; Thekdi, Arvind; Keiser, James R; Storey, John Morse

    2015-01-01

    This article describes electric arc furnace (EAF) off-gas enthalpy models developed at Oak Ridge National Laboratory (ORNL) to calculate overall heat availability (sensible and chemical enthalpy) and recoverable heat values (steam or power generation potential) for existing EAF operations and to test ORNL s new EAF waste heat recovery (WHR) concepts. ORNL s new EAF WHR concepts are: Regenerative Drop-out Box System and Fluidized Bed System. The two EAF off-gas enthalpy models described in this paper are: 1.Overall Waste Heat Recovery Model that calculates total heat availability in off-gases of existing EAF operations 2.Regenerative Drop-out Box System Model in which hot EAF off-gases alternately pass through one of two refractory heat sinks that store heat and then transfer it to another gaseous medium These models calculate the sensible and chemical enthalpy of EAF off-gases based on the off-gas chemical composition, temperature, and mass flow rate during tap to tap time, and variations in those parameters in terms of actual values over time. The models provide heat transfer analysis for the aforementioned concepts to confirm the overall system and major component sizing (preliminary) to assess the practicality of the systems. Real-time EAF off-gas composition (e.g., CO, CO2, H2, and H2O), volume flow, and temperature data from one EAF operation was used to test the validity and accuracy of the modeling work. The EAF off-gas data was used to calculate the sensible and chemical enthalpy of the EAF off-gases to generate steam and power. The article provides detailed results from the modeling work that are important to the success of ORNL s EAF WHR project. The EAF WHR project aims to develop and test new concepts and materials that allow cost-effective recovery of sensible and chemical heat from high-temperature gases discharged from EAFs.

  10. Polychlorinated naphthalene (PCN) emissions from scrap processing steel plants with electric-arc furnaces.

    PubMed

    Odabasi, Mustafa; Dumanoglu, Yetkin; Kara, Melik; Altiok, Hasan; Elbir, Tolga; Bayram, Abdurrahman

    2017-01-01

    Polychlorinated naphthalene (PCN) emissions of scrap iron processing steel plants were explored by measuring concentrations in stack gases of five plants, in the atmosphere (n=11) at a site close to those plants, and in soil at several sites in the region (n=40) in Aliaga, Izmir, Turkey. Observed stack-gas Σ32PCN levels from the plants without scrap preheating (189±157ngNm(-3), average±SD, n=4) showed that they are substantial PCN emitting sources. Stack-gas Σ32PCN level for the plant with scrap preheating was considerably higher (1262ngNm(-3)). Similarly, Σ32PCN emission factor for this plant was substantially higher (11.9mgton(-1)) compared to those without scrap preheating (1.30±0.98mgton(-1)). Results have also suggested that the investigated steel plants emit large quantities of fugitive particle-phase PCNs. Measured soil Σ32PCN concentrations that are considered to be representative of the atmospheric levels were greatly variable in the region, ranging between 0.003 and 10.02μgkg(-1) (dry wt). Their spatial distribution showed that main PCN sources in the region were the iron-steel plants. Ambient air levels (1620±800pgm(-3)) were substantially higher than ones observed around the world and in the study area verifying that the steel plants with electric arc furnaces (EAFs) are important PCN sources. Investigation of possible mechanisms suggested that the combustion processes also contribute to emissions from EAFs in addition to evaporation of PCNs present in the scrap iron.

  11. Solidification/stabilisation of electric arc furnace waste using low grade MgO.

    PubMed

    Cubukcuoglu, B; Ouki, S K

    2012-02-01

    This study aims to evaluate the potential of low grade MgO (LGMgO) for the stabilisation/solidification (S/S) of heavy metals in steel electric arc furnace wastes. Relevant characteristics such as setting time, unconfined compressive strength (UCS) and leaching behaviour assessed by acid neutralisation capacity (ANC), monolithic and granular leaching tests were examined in light of the UK landfill Waste Acceptance Criteria (WAC) for disposal. The results demonstrated that all studied mix designs with Portland cement type 1 (CEM1) and LGMgO, CEM1-LGMgO 1:2 and 1:4 at 40% and 70% waste addition met the WAC requirements by means of UCS, initial and final setting times and consistence. Most of the ANC results met the WAC limits where the threshold pH values without acid additions were stable and between 11.9 and 12.2 at 28d. Granular leaching results indicate fixation of most of the metals at all mix ratios. An optimum ratio was obtained at CEM1-LGMgO 1:4 at 40% waste additions where none of the metals leaching exceeded the WAC limits and hence may be considered for landfill disposal. The monolithic leaching test results showed that LGMgO performed satisfactorily with respect to S/S of Zn, as the metal component present at the highest concentration level in the waste exhibited very little leaching and passed the leaching test requirement at all mix ratios studied. However, its performance with respect to Pb, Cd and Cr was less effective in reducing their leaching suggesting a higher cumulative rate under those leaching regimes.

  12. Long and short-term performance of a stabilized/solidified electric arc furnace dust.

    PubMed

    Pereira, C Fernández; Galiano, Y Luna; Rodríguez-Piñero, M A; Parapar, J Vale

    2007-09-30

    The application of class F fly ash, cement and lime to the Stabilization/Solidification (S/S) of electric arc furnace dust containing hazardous metals such as Zn, Pb, Cd, and Cr is described. The aim of the study was to determine the influence of the setting conditions during the S/S treatment and to know the behaviour of an aged solidified and stabilized waste. In order to determine the efficiency attained by the S/S process, USEPA TCLP, and other leaching tests have been accomplished. In addition, the compressive strength of the solidified waste at different times has been determined. In order to study the influence of the environmental conditions in which setting occurs, experiments were carried out with samples of the same composition, under different setting conditions: laboratory environment, stove at a temperature of 40-60 degrees C and setting in a hermetically sealed plastic bag at room temperature. All the samples were subjected to the TCLP test at 28 days, and the metal content of the resulting leachates was analysed. The results show that in some cases the setting conditions of the mixtures have a noticeable influence on the characteristics of the leachate. The evolution with time of some S/S solids, one month after their manufacture and more than 9 years after that has also been evaluated, by means of their leaching behaviour. The results obtained in this work have shown, in all the laboratory cured samples that the leachate pH decrease in the course of time, and consequently the leaching behaviour is in general worse. This could be due to the carbonation of the S/S solid and the subsequent loss of alkalinity.

  13. Evaluation of the emission characteristics of PCDD/Fs from electric arc furnaces.

    PubMed

    Chang, Moo Been; Huang, Hung Chi; Tsai, Shian Sheng; Chi, Kai Hsien; Chang-Chien, Guo Ping

    2006-03-01

    Distribution of PCDD/F (polychlorinated dibenzo-p-dioxin and polychlorinated dibenzofuran) congeners at two electric arc furnaces (EAFs) in Taiwan is evaluated via intensive stack sampling and analysis. Two kinds of exhaust system in EAFs including stack system and shutter system are selected for measuring dioxin emissions. In addition, dioxin emissions during oxidation and reduction stages at EAF-A were characterized. Results indicate that the PCDD/F concentration of stack gas in EAF-A was 4.39 ng/Nm(3) while total Toxic Equivalent Quantity (TEQ) concentration was 0.35 ng I-TEQ/Nm(3). The PCDD/F concentration of stack gas in EAF-B was 2.20 ng/Nm(3) and the TEQ concentration was 0.14 ng I-TEQ/Nm(3). 1,2,3,4,6,7,8-H(p)CDF, OCDD and OCDF are the major contributors of the dioxin concentrations for two EAFs investigated and the percentage of PCDD/F in particulate phase increases as the chlorination level of the PCDD/F congener increases. The results obtained on gas/particulate partitioning of PCDD/Fs in flue gases prior to the APCD in EAFs indicate that more than 90% exists in particulate phase. In EAF-A, the PCDD/F concentration during oxidation stage is slightly higher than that measured during reduction stage, including the sampling points of CO converter outlet, prior to bag filter and stack. Majority of PCDD/Fs emitted from steel-making processes exists in particulate-phase (about 60-70%) at both EAFs investigated.

  14. [Phosphorus adsorption and regeneration of electric arc furnace steel slag as wetland medium].

    PubMed

    Zhai, Li-hua; He, Lian-sheng; Xi, Bei-dou; Chen, Yue; Meng, Rui; Huo, Shou-liang; Liu, Hong-liang

    2008-12-01

    The long-term phosphorus (P) adsorption and retention capacities of electric arc furnace (EAF) steel slag materials derived from one batch and a 278-d column experiments with a synthetic P solution were compared. The investigations of the regeneration of the P adsorption capacity by water level decrease was conducted. It was revealed column experiment on a long-term basis can determine P saturation of EAF accurately. And the results can be used for realistic estimations of constructed wetland systems (CWS) longevity. EAF slag showed a high afinity for P, reaching a saturation value of 1.65 g/kg. Regeneration experiment of the P adsorbing capacity by this material showed that, after 4 weeks of water level decrease, EAF steel slag was able to increase its initial P adsorption capacity to 2.65 g/kg. A sequential P fractionation experiment was performed to quantify the proportion of P bound to mineral compounds in EAF. From the most loosely bound to the most strongly bound P fraction, P1 was associated with resin extractable (13%), Fe extractable (0.5 mol/L Na2CO3, 39%), Al extractable (0.1 mol/L NaOH, 21%), Ca extractable (1 mol/L HCl, 13%), and Ca in a stable residual pool (concentrated hot HCl, 14%). X-ray fluorescence analyses of EAF steel slag chemical composition revealed that the continuous application of a P solution resulted in 300% and 170% increases in K2O and P2O5, respectively. Al2O3 and FeO increased by 8%, while the portion of CaO remained unchanged. The investigated properties (P retention potential, regeneration of P adsorption, P fractionation) provide useful data about the suitability of slag material as a media for longterm P removal and dry-wet operation can improve P retention capacity of EAF to prolong the longevity of full-scale CWS.

  15. Identification and characterization of the atmospheric emission of polychlorinated naphthalenes from electric arc furnaces.

    PubMed

    Liu, Guorui; Zheng, Minghui; Du, Bing; Nie, Zhiqiang; Zhang, Bing; Hu, Jicheng; Xiao, Ke

    2012-09-01

    Electric arc furnaces (EAF) are well recognized as significant sources of dioxins. EAFs have also been speculated to be sources of polychlorinated naphthalenes (PCNs) due to the close correlation between dioxin and PCN formation. However, assessment on PCN emissions from EAFs has not been carried out. The primary aim of this preliminary study is to identify and characterize the atmospheric emission of PCNs from EAFs. In this preliminary study, stack gas samples from two typical EAFs with different scales (EAF-1, 160 t batch(-1); and EAF-2, 60 t batch(-1)) were collected by automatic isokinetic sampling technique, and PCN congeners in samples were analyzed by isotope dilution high-resolution gas chromatography combined with high-resolution mass spectrometry method. Emission concentrations of PCNs were 458 and 1,099 ng m(-3) for EAF-1 and EAF-2, respectively. The emission factors of PCNs to air were 21.6 and 30.1 ng toxic equivalent t(-1) for EAF-1 and EAF-2, respectively, which suggested that EAF is an important source of PCN release. With regard to the characteristics of PCNs from EAFs, lower chlorinated homologues were dominant. The PCN congeners comprised of CN27/30, CN52/60, CN66/67, and CN73 were the most abundant congeners for tetra-, penta-, hexa-, and hepta-chlorinated homologues, respectively. EAFs were identified to be an important PCN source, and the obtained data are useful for developing a PCN inventory. The congener profiles of PCNs presented here might provide helpful information for identifying the specific sources of PCNs emitted from EAFs.

  16. Recycling of rubber tires in electric arc furnace steelmaking: simultaneous combustion of metallurgical coke and rubber tyres blends

    SciTech Connect

    Magdalena Zaharia; Veena Sahajwalla; Byong-Chul Kim; Rita Khanna; N. Saha-Chaudhury; Paul O'Kane; Jonathan Dicker; Catherine Skidmore; David Knights

    2009-05-15

    The present study investigates the effect of addition of waste rubber tires on the combustion behavior of its blends with coke for carbon injection in electric arc furnace steelmaking. Waste rubber tires were mixed in different proportions with metallurgical coke (MC) (10:90, 20:80, 30:70) for combustion and pyrolysis at 1473 K in a drop tube furnace (DTF) and thermogravimetric analyzer (TGA), respectively. Under experimental conditions most of the rubber blends indicated higher combustion efficiencies compared to those of the constituent coke. In the early stage of combustion the weight loss rate of the blends is much faster compared to that of the raw coke due to the higher volatile yield of rubber. The presence of rubber in the blends may have had an impact upon the structure during the release and combustion of their high volatile matter (VM) and hence increased char burnout. Measurements of micropore surface area and bulk density of the chars collected after combustion support the higher combustion efficiency of the blends in comparison to coke alone. The surface morphology of the 30% rubber blend revealed pores in the residual char that might be attributed to volatile evolution during high temperature reaction in oxygen atmosphere. Physical properties and VM appear to have a major effect upon the measured combustion efficiency of rubber blends. The study demonstrates that waste rubber tires can be successfully co-injected with metallurgical coke in electric arc furnace steelmaking process to provide additional energy from combustion. 44 refs., 11 figs., 2 tabs.

  17. In vitro assessment of genotoxic effects of electric arc furnace dust on human lymphocytes using the alkaline comet assay.

    PubMed

    Garaj-Vrhovac, Vera; Orescanin, Visnja; Ruk, Damir; Gajski, Goran

    2009-02-15

    In vitro genotoxic effects of leachates of electric arc furnace dust (EAFD) on human peripheral lymphocytes, assessed prior and following the treatment with a strong alkaline solution were investigated using the alkaline comet assay. Prior and following the treatment, lymphocytes were incubated with leachate of EAFD for 6 and 24 hours at 37 degrees C. Negative controls were also included. Mean values of the tail lengths established in the samples treated with the leachate stemming from the original dust for 6 and 24 hours, were 15.70 microm and 16.78 microm, respectively, as compared to 12.33 microm found in the control sample. Slight, but significant increase in the tail length was also found with the dust treated with a strong alkaline solution (13.37 microm and 13.60 microm). In case of high heavy metal concentrations (the extract of the original furnace dust), the incubation period was revealed to be of significance as well. The obtained results lead to the conclusion that alkaline comet assay could be used as a rapid, sensitive and low-cost tool when assessing genotoxicity of various waste materials, such as leachates of the electric arc furnace dust.

  18. Chlorine determination via MgCl molecule in environmental samples using high resolution continuum source graphite furnace molecular absorption spectrometry.

    PubMed

    Medeiros, Rina Lourena da S; Souza, Sidnei Oliveira; Araújo, Rennan Geovanny Oliveira; da Silva, Djalma Ribeiro; Maranhão, Tatiane de A

    2018-01-01

    This paper describes a method development for chlorine determination through the formation of MgCl molecule, applied for the first time for Cl quantification, by high resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) in environmental samples. Pyrolysis and vaporization temperatures were optimized as well as the use of chemical modifier. Determinations were carried out at the wavelength of 377.010 and the compromise conditions of the graphite furnace temperature program were 500°C and 2500°C for pyrolysis and vaporization, respectively, using 10µg of chemical modifier Pd. The concentration of reactants for the generation of MgCl molecule was optimized through Box-Behnken experimental design, using MgCl2 solution as source of chlorine. The optimum values according to the surface response were 5gL(-1) Mg, 25mgL(-1) of chlorine and 2% vv(-1) of HNO3, condition in which the amount of Mg is at least 200 times higher than that of chloride. This excess of the forming agent ensures the complete formation of MgCl molecular species, since Cl is the limiting reactant. Certified reference materials, BCR 182 and NIST 8414, and addition and recovery tests were used to evaluate the accuracy of the method and good results were achieved at a 95% confidence level. The method was applied to direct determination of Cl in five produced water samples from offshore oil wellbore, high complex matrix, whose conventional methods require tedious treatment before the analysis. Copyright © 2017. Published by Elsevier B.V.

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

    USGS Publications Warehouse

    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.

  20. Tungsten permanent chemical modifier for fast estimation of Se contents in soil by graphite furnace atomic absorption spectrometry.

    PubMed

    Rosa, Cassia Regina; Freschi, GianPaulo Giovanni; De Moraes, Mercedes; Gomes Neto, José Anchieta; Nóbrega, Joaquim Araújo; Araújo Nogueira, Ana Rita; Sacramento, Luís Vitor

    2003-07-02

    A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer was used as a modifier for the direct determination of Se in soil extracts by graphite furnace atomic absorption spectrometry. Diethylenetriaminepentaacetic acid (0.0050 mol L(-1)) plus ammonium hydrogencarbonate (1.0 mol L(-1)) extracted predominantly available inorganic selenate from soil. The formation of a large amount of carbonaceous residue inside the atomizer was avoided with a first pyrolysis step at 600 degrees C assisted by air during 30 s. For 20 microL of soil extracts delivered to the atomizer and calibration by matrix matching, an analytical curve (10.0-100 microgram of L(-1)) with good linear correlation (r = 0.999) between integrated absorbance and analyte concentration was established. The characteristic mass was approximately 63 pg of Se, and the lifetime of the tube was approximately 750 firings. The limit of detection was 1.6 microgram L(-1), and the relative standard deviations (n = 12) were typically <4% for a soil extract containing 50 microgram of L(-1). The accuracy of the determination of Se was checked for soil samples by means of addition/recovery tests. Recovery data of Se added to four enriched soil samples varied from 80 to 90% and indicated an accurate method.

  1. Evaluation of ammonia as diluent for serum sample preparation and determination of selenium by graphite furnace atomic absorption spectrometry*1

    NASA Astrophysics Data System (ADS)

    Hernández-Caraballo, Edwin A.; Burguera, Marcela; Burguera, José L.

    2002-12-01

    A method for the determination of total selenium in serum samples by graphite furnace atomic absorption spectrometry was evaluated. The method involved direct introduction of 1:5 diluted serum samples (1% v/v NH 4OH+0.05% w/v Triton X-100 ®) into transversely heated graphite tubes, and the use of 10 μg Pd+3 μg Mg(NO 3) 2 as chemical modifier. Optimization of the modifier mass and the atomization temperature was conducted by simultaneously varying such parameters and evaluating both the integrated absorbance and the peak height/peak area ratio. The latter allowed the selection of compromise conditions rendering good sensitivity and adequate analyte peak profiles. A characteristic mass of 49 pg and a detection limit (3s) of 6 μg 1 -1 Se, corresponding to 30 μg l -1 Se in the serum sample, were obtained. The analyte addition technique was used for calibration. The accuracy was assessed by the determination of total selenium in Seronorm™ Trace Elements Serum Batch 116 (Nycomed Pharma AS). The method was applied for the determination of total selenium in ten serum samples taken from individuals with no known physical affection. The selenium concentration ranged between 79 and 147 μg l -1, with a mean value of 114±22 μg l -1.

  2. Temporal variations in gas temperature in an atomization stage of cadmium and tellurium evaluated by using the two-line method in graphite furnace atomic absorption spectrometry.

    PubMed

    Shimabukuro, Haruki; Ashino, Tetsuya; Wagatsuma, Kazuaki

    2008-09-01

    In order to discuss the atomization process of an analyte element occurring in a graphite furnace for atomic absorption spectrometry, we measured variations in the characteristic temperature with the progress of an atomization stage, by using a two-line method under the assumption of a Boltzmann distribution. For this purpose, iron was chosen as the analyte element. Also, the atomic absorption of two iron atomic lines, Fe I 372.0 nm and Fe I 373.7 nm, was simultaneously monitored as a probe for the temperature determination. This method enables variations in the gas temperature to be directly traced, yielding a temperature distribution closely related to the diffusion behavior of the probe element in the furnace. This temperature variation was very different from the furnace wall temperatures, which were monitored in conventional temperature control for atomic absorption spectrometry. Correlations between the gas temperature and the charring/atomizing temperatures in the heating program of the furnace were investigated. The atomization of cadmium and tellurium was also investigated by a comparison between the gas temperature with the wall temperature of the furnace. The atomic absorption of cadmium or tellurium appeared to be apart from the absorption of iron while the gas temperature was still low. Therefore, the analyte atoms could be atomized through direct contact with the wall of the graphite furnace, which has a much higher temperature compared to the gas atmosphere during atomization. Their atomization would be caused by conductive heating from the furnace wall rather than by radiant heating in the furnace.

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

    PubMed

    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.

  4. Health status of male steel workers at an electric arc furnace (EAF) in Trentino, Italy.

    PubMed

    Cappelletti, Roberto; Ceppi, Marcello; Claudatus, Justina; Gennaro, Valerio

    2016-01-01

    The aim of this retrospective cohort study was to determine if the workers of an Electric Arc Furnace (EAF), which recycles scrap, had higher mortality and morbidity due to possible exposure to pollutants at work. EAFs do not run on coke ovens. In EAFs 40 % of the particulate matter (PM) is made up of PM 2.5. The foundry dust contained iron, aluminum, zinc, manganese, lead, chromium, nickel, cadmium, mercury, arsenic, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls and dioxins. Mortality study: a cohort of 331 exposed workers (6731 person-years) was studied from 19/03/1979 to 31/12/2009 (mean follow up 20.7 years). The group of exposed workers was compared to the general population and to a small control group of 32 workers from the same company. Morbidity study: rates of exemption from health fee for the seven major diseases of 235 exposed workers were compared to the rates of exemption in the Province of Trento. Mortality study: an excess mortality was found in the exposed workers as compared to the general population (SMR 1.13; 95 % CI: 0.76-1.62; 29 deaths) and to the internal group (RR 2.34; 95 % CI: 0.39-95.7). The mortality rate was increased for all tumours (SMR 1.36; 95 % CI: 0.75-2.29; 14 cases), for lung cancer (SMR 3.35; 95 % CI 1.45-6.60; 8 cases), for ischemic heart disease (SMR 1.27; 95 % CI: 0.35-3.26; 4 cases), for chronic liver disease (SMR 1.16; 95 % CI: 0.14-4.20; 2 cases) and for injury and poisoning (SMR 1.32; 95 % CI: 0.48-2.88; 6 cases). Morbidity study: there was a statistically significant increase of diabetes, rheumatoid arthritis, hypertension and cardiovascular diseases in exposed workers. With the limitations of this relatively small cohort, we found a statistically significant increase of diabetes, cardiovascular diseases and deaths due to lung cancer in exposed workers. These findings cannot be explained by PAH exposure alone; metal particulates are the most important pollutants in the working area of EAFs

  5. Recycling of Malaysia's electric arc furnace (EAF) slag waste into heavy-duty green ceramic tile.

    PubMed

    Teo, Pao-Ter; Anasyida, Abu Seman; Basu, Projjal; Nurulakmal, Mohd Sharif

    2014-12-01

    Recently, various solid wastes from industry such as glass waste, fly ash, sewage sludge and slag have been recycled into various value-added products such as ceramic tile. The conventional solutions of dumping the wastes in landfills or incineration, including in Malaysia are getting obsolete as the annual huge amount of the solid wastes would boost-up disposal cost and may cause permanent damage to the flora and fauna. This recent waste recycling approach is much better and greener as it can resolve problems associated with over-limit storage of industrial wastes and reduce exploration of natural resources for ceramic tile to continuously sustain the nature. Therefore, in this project, an attempt was made to recycle electric arc furnace (EAF) slag waste, obtained from Malaysia's steel making industry, into ceramic tile via conventional powder compaction method. The research work was divided into two stages. The first stage was to evaluate the suitability of EAF slag in ceramic tile by varying weight percentage of EAF slag (40 wt.%, 50 wt.% and 60 wt.%) and ball clay (40 wt.%, 50 wt.% and 60 wt.%), with no addition of silica and potash feldspar. In the second stage, the weight percentage of EAF slag was fixed at 40 wt.% and the percentage of ball clay (30 wt.% and 40 wt.%), feldspar (10 wt.% and 20 wt.%) and silica (10 wt.% and 20 wt.%) added was varied accordingly. Results obtained show that as weight percentage of EAF slag increased up to 60 wt.%, the percentage of apparent porosity and water absorption also rose, with a reduction in tile flexural strength and increased porosity. On the other hand, limiting the weight percentage of EAF slag to 40 wt.% while increasing the weight percentage of ball clay led to a higher total percentage of anorthite and wollastonite minerals, resulting in higher flexural strength. It was found that introduction of silica and feldspar further improved the flexural strength due to optimization of densification process. The highest

  6. Investigations on phosphorus recovery and reuse as soil amendment from electric arc furnace slag filters.

    PubMed

    Bird, Simon C; Drizo, Aleksandra

    2009-11-01

    Electric arc furnace (EAF) steel slag has been identified as an effective filter material for the removal of phosphorus (P) from both point and non-point sources. To determine the feasibility of land-applying P saturated EAF steel slag this study was undertaken to investigate (i) saturated EAF steel slag material's potential as a P fertilizer or soil amendment and (ii) P desorption and metals leachate from saturated EAF steel slag material to surface runoff. Medicago sativa (alfalfa) was planted in a nutrient depleted washed sand media. Phosphorus was added either as saturated EAF steel slag or as a standard commercial phosphate fertilizer in order to assess the plant availability of the P from saturated EAF steel slag. Four different P application levels were tested: a low (20 lbs acre furrow slice(-1) (5.5 g P m(-3))) two medium (40 and 60 lbs. acre f.s.(-1) (11 and 16.5 g P m(-3))) and a high (120 lbs. acre f.s.(-1) (33 g P m(-3))). The above-ground biomass of half of the plants was harvested after 5 weeks and the second half at 10 weeks. All treatments regardless of the P source used showed high rates of germination. At the first harvest period (5 weeks) significantly higher above-ground biomass (p < 0.01) was seen at the 3 highest P amendment rates in treatments with triple super phosphate fertilizer (TSP) than with EAF steel slag. However, by the second harvest (10 weeks) only the highest amendment rate of TSP showed a significantly higher amount of biomass (p < 0.01), suggesting that EAF steel slag might be an effective slow release P source. In a second experiment, a rain simulator was used to assess desorption of DRP, TP and metals from a saturated and semi-saturated EAF steel slag. The results revealed that the total amounts of DRP and TP released to surface runoff from EAF steel slag were negligible when compared to the total quantities of P retained by this material. Overall the results from this study demonstrated that once the EAF steel slag filter

  7. Physics-Based Modeling of Electric Operation, Heat Transfer, and Scrap Melting in an AC Electric Arc Furnace

    NASA Astrophysics Data System (ADS)

    Opitz, Florian; Treffinger, Peter

    2016-04-01

    Electric arc furnaces (EAF) are complex industrial plants whose actual behavior depends upon numerous factors. Due to its energy intensive operation, the EAF process has always been subject to optimization efforts. For these reasons, several models have been proposed in literature to analyze and predict different modes of operation. Most of these models focused on the processes inside the vessel itself. The present paper introduces a dynamic, physics-based model of a complete EAF plant which consists of the four subsystems vessel, electric system, electrode regulation, and off-gas system. Furthermore the solid phase is not treated to be homogenous but a simple spatial discretization is employed. Hence it is possible to simulate the energy input by electric arcs and fossil fuel burners depending on the state of the melting progress. The model is implemented in object-oriented, equation-based language Modelica. The simulation results are compared to literature data.

  8. [Determination of beryllium in river water by graphite furnace atomic absorption spectrometry].

    PubMed

    Sun, X

    1999-08-01

    The graphite tube such as Lanthanum-coated or Barium-coated have been tested for the determination of Be in water by GFAAS. The effects of different metal ions have been eliminated by adding Al (III) or Ca (III) as matrix modifier. The method is handy and fast. The recovery is 92.6%-105.0% and RSD is less than 10.24%.

  9. Leaching behavior of pollutants in ferrochrome arc furnace dust and its stabilization/solidification using ferrous sulphate and Portland cement.

    PubMed

    Bulut, Ulkü; Ozverdi, Arzu; Erdem, Mehmet

    2009-03-15

    In this study, dissolution properties under different conditions and pollution potential by toxicity characteristic leaching procedure (TCLP) of arc furnace dust generated in the production of ferrochrome were examined and some stabilization/solidification (S/S) techniques were applied to the dust depending on contaminants determined. Dissolution properties and pollution potentials of all the materials stabilized/solidified were also studied under the similar conditions. It was determined that the metallic components concentrations dissolved from the ferrochrome arc furnace dust (FAFD) except for chromium and zinc were below the detection limits. The chromium concentration dissolved from the FAFD by TCLP was found to be 9.8 mg/l. Portland cement (PC), PC-FeSO(4) and PC-sand-FeSO(4) mixtures for S/S of the FAFD were tested. Although metal ions in the cationic form were stabilized when the PC was only used, Cr(VI) in the sample was not changed depending on PC amount and remained in the soluble chromate form. The stabilization efficiency of Cr(VI) increased by the increasing amounts of PC and FeSO(4). The best S/S of the FAFD was accomplished when the 5 stoichiometric amounts of FeSO(4), 30% PC and 16% sand mixture were used. TCLP leaching results of the samples obtained under the optimum conditions were below the EPA landfilling limits.

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

    PubMed

    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.

  11. Optimization of high-resolution continuum source graphite furnace atomic absorption spectrometry for direct analysis of selected trace elements in whole blood samples.

    PubMed

    Wójciak-Kosior, Magdalena; Szwerc, Wojciech; Strzemski, Maciej; Wichłacz, Zoltan; Sawicki, Jan; Kocjan, Ryszard; Latalski, Michał; Sowa, Ireneusz

    2017-04-01

    Trace analysis plays an important role in medicine for diagnosis of various disorders; however, the appropriate sample preparation is required mostly including mineralization. Although graphite furnace atomic absorption spectrometry (GF AAS) allows the investigation of biological samples such as blood, serum, and plasma without this step, it is rarely used for direct analysis because the residues of the rich organic matrix inside the furnace are difficult to remove and this may cause spectral/matrix interferences and decrease the lifetime of the graphite tube. In our work, the procedure for determination of Se, Cr, Mn, Co, Ni, Cd and Pb with the use of the high resolution continuum source GF-AAS technique in whole blood samples with minimum sample pre-treatment was elaborated. The pyrolysis and atomization temperature as well as the time of signal integration were optimized to obtain the highest intensity and repeatability of the analytical signal. Moreover, due to the apparatus modification, an additional step was added in the for graphite furnace temperature program with minimal argon flow and maximal flow of air during pyrolysis stage to increase the oxidative condition for better matrix removal. The accuracy and precision of the optimized method was verified using certified reference material (CRM) Seronorm Trace Elements Whole Blood L-1 and the developed method was applied for trace analysis of blood samples from volunteer patients of the Orthopedics Department. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    PubMed

    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. Graphite furnace atomic absorption spectrometry as a routine method for the quantification of beryllium in blood and serum

    PubMed Central

    Stephan, Chadi H; Fournier, Michel; Brousseau, Pauline; Sauvé, Sébastien

    2008-01-01

    Background A routine method for the quantification of beryllium in biological fluids is essential for the development of a chelation therapy for Chronic Beryllium Disease (CBD). We describe a procedure for the direct determination of beryllium in undigested micro quantities of human blood and serum using graphite furnace atomic absorption spectrometry. Blood and serum samples are prepared respectively by a simple 8-fold and 5-fold dilution with a Nash Reagent. Three experimental setups are compared: using no modifier, using magnesium nitrate and using palladium/citric acid as chemical modifiers. Results In serum, both modifiers did not improve the method sensitivity, the optimal pyrolysis and atomization temperatures are 1000°C and 2900°C, respectively. In blood, 6 μg of magnesium nitrate was found to improve the method sensitivity. The optimal pyrolysis and atomization temperatures were 800°C and 2800°C respectively. Conclusion In serum, the method detection limit was 2 ng l-1, the characteristic mass was 0.22 (± 0.07) pg and the accuracy ranged from 95 to 100%. In blood, the detection limit was 7 ng l-1, the characteristic mass was 0.20 (± 0.02) pg and the accuracy ranged from 99 to 101%. PMID:18597692

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

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

    2014-01-01

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

  17. Determination of cadmium and lead in beverages after leaching from pewter cups using graphite furnace atomic absorption spectrometry.

    PubMed

    Dessuy, Morgana B; Vale, Maria Goreti R; Welz, Bernhard; Borges, Aline R; Silva, Márcia M; Martelli, Patrícia B

    2011-07-15

    Two simple methods have been developed to determine cadmium and lead in different kinds of beverages and vinegar leached from pewter cups produced in Brazil. Leaching experiments have been carried out with different solutions: beer, sugar cane spirit, red and white wine, vinegar and a 3% acetic acid solution. The solutions were kept in cups with and without solder for 24h. Lead and cadmium have been determined using graphite furnace atomic absorption spectrometry with deuterium background correction. The limits of detection were 0.05 and 1.4 μg L(-1), and the characteristic mass was 1.0 pg and 19 pg for Cd and Pb, respectively. With the developed methods it was possible to determine accurately cadmium and lead by direct analysis in these liquids and to evaluate the leaching of these metals from pewter cups. The results presented in this work show that pewter cups are not cadmium- and lead-free; this point goes against the manufacturers' declaration that their products are lead-free. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    PubMed

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

    2013-03-30

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

  19. Analysis of lead in 55 brands of dietary calcium supplements by graphite furnace atomic absorption spectrometry after microwave digestion.

    PubMed

    Kim, Meehye; Kim, Changmin; Song, Insang

    2003-02-01

    The lead (Pb) contents of calcium (Ca) supplements available in Korea were determined by graphite furnace atomic absorption spectrometry using Zeeman background correction and peak area mode. All samples were microwave-digested in concentrated HNO(3). Ammonium dihydrogen phosphate and magnesium nitrate were used as matrix modifiers. Fifty-five brands of Ca supplements were classified into seven categories based on the major composite: bone, milk, oyster/clam shell, egg shell, algae, shark cartilage and chelated. The mean Pb contents of Ca supplements were 1.1 microg g(-1) (coefficient of variation 5.7%), ranging from n.d. (not detected) to 6.7 microg g(-1). Ca supplements made of bone have the highest Pb contents (2.3 microg g(-1)) with a wide range (0.1-6.7 microg g(-1)). The results were similar to those reported in other countries. The mean daily intakes of Pb from the supplement could be about 5 microg (mean Pb concentration 1.1 microg g(-1) x mean daily intake 4.5 g) taking 2% of provisional tolerable daily intake that the FAO/WHO Joint Food Additive and Contaminants Committee has set to evaluate its safety. However, measures to prevent potentials of Pb toxicity from overtaking some Ca supplements should be considered.

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

    NASA Astrophysics Data System (ADS)

    Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R.; Welz, Bernhard; Carasek, Eduardo; de Andrade, Jailson B.

    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%).

  1. Morphological study of graphite-encapsulated iron composite nanoparticles fabricated by a one-step arc discharge method

    NASA Astrophysics Data System (ADS)

    Hu, Rui; Furukawa, Taiki; Wang, Xiangke; Nagatsu, Masaaki

    2017-09-01

    Arc discharge is one of the most efficient approaches to fabricate graphite-encapsulated magnetic nanoparticles. However, given the ultra-fast synthetic procedure, the understanding of tailoring shell morphology and quality over magnetic core has been a long standing challenge. To better comprehend the mechanism of the encapsulating shell growth in plasma, a series of synthetic parameters were investigated systematically in this study. Specifically, (1) the surface morphology of the outmost shell evolved with high integrity by adding CH4 concentration from 0% to 50% to He background gas; (2) a smooth surface with higher graphitization degree was achieved by changing collecting zone closer to the arc center; (3) carbon nano loops on the outmost shell expanded volumetrically to be continuous amorphous cover as the working gas pressure decreases from 100 to 25 Torr. The surface properties (i.e., zeta potential and acid-base character) were also evaluated and explained through XPS technique.

  2. Slurry sampling graphite furnace atomic absorption spectrometry: determination of trace metals in mineral coal.

    PubMed

    Silva, M M; Goreti, M; Vale, R; Caramão, E B

    1999-12-06

    A procedure for lead, cadmium and copper determination in coal samples based on slurry sampling using an atomic absorption spectrometer equipped with a transversely heated graphite tube atomizer is proposed. The slurries were prepared by weighing the samples directly into autosampler cups (5-30 mg) and adding a 1.5 ml aliquot of a diluent mixture of 5% v/v HNO(3), 0.05% Triton X-100 and 10% ethanol. The slurry was homogenized by manual stirring before measurement. Slurry homogenization using ultrasonic agitation was also investigated for comparison. The effect of particle size and the use of different diluent compositions on the slurry preparation were investigated. The temperature programmes were optimized on the basis of pyrolysis and atomization curves. Absorbance characteristics with and without the addition of a palladium-magnesium modifier were compared. The use of 0.05% m/v Pd and 0.03% m/v Mg was found satisfactory for stabilizing Cd and Pb. The calibration was performed with aqueous standards. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling. Better recoveries of the analytes were obtained when the particle size was reduced to <37 mum. Several certified coal reference materials (BCR Nos. 40, 180, and 181) were analyzed, and good agreement was obtained between the results from the proposed slurry sampling method and the certificate values.

  3. Development of an analytical method for the determination of arsenic in gasoline samples by hydride generation-graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Becker, Emilene M.; Dessuy, Morgana B.; Boschetti, Wiliam; Vale, Maria Goreti R.; Ferreira, Sérgio L. C.; Welz, Bernhard

    2012-05-01

    The purpose of the present work was to optimize the conditions for the determination of arsenic in gasoline with hydride generation-graphite furnace atomic absorption spectrometry after acid digestion using a full two-level factorial design with center point. The arsine was generated in a batch system and collected in a graphite tube coated with 150 μg Ir as a permanent modifier. The sample volume, the pre-reduction conditions, the temperature program and modifier mass were kept fixed for all experiments. The estimated main effects were: reducing agent concentration (negative effect), acid concentration (negative effect) and trapping temperature (positive effect). It was observed that there were interactions between the variables. Moreover, the curvature was significant, indicating that the best conditions were at the center point. The optimized parameters for arsine generation were 2.7 mol L- 1 hydrochloric acid and 1.6% (w/v) sodium tetrahydroborate. The optimized conditions to collect arsine in the graphite furnace were a trapping temperature of 250 °C and a collection time of 30 s. The limit of detection was 6.4 ng L- 1 and the characteristic mass was 24 pg. Two different systems for acid digestion were used: a digester block with cold finger and a microwave oven. The concentration of arsenic found with the proposed method was compared with that obtained using a detergentless microemulsion and direct graphite furnace determination. The results showed that the factorial design is a simple tool that allowed establishing the appropriate conditions for sample preparation and also helped in evaluating the interaction between the factors investigated.

  4. Innovative Concept for the Recovery of Silver and Indium by a Combined Treatment of Jarosite and Electric Arc Furnace Dust

    NASA Astrophysics Data System (ADS)

    Wegscheider, S.; Steinlechner, S.; Leuchtenmüller, M.

    2016-11-01

    Industrial wastes such as slags, dust, or precipitation residues contain significant amounts of valuable metals like zinc, lead, and copper as well as precious metals like silver and indium. Nevertheless, a lot of these waste materials are not recycled, and therefore, many valuable metals end up being sent to landfills. Because of harmful components in the waste, it is often necessary to send it to specialized landfills for hazardous wastes, which leads to environmental problems as well as additional costs. Consequently, the recovery of the valuable metals from the residues represents a sensible task to decrease the negative impact on the environment and to reduce costs for maintaining a landfill. In addition, recycling helps to decrease the dependency from primary resources. The present study deals with the behavior of different metals in a pyro-metallurgical treatment for a mixture of jarosite and electric arc furnace dust with a special focus on indium and silver.

  5. Innovative Concept for the Recovery of Silver and Indium by a Combined Treatment of Jarosite and Electric Arc Furnace Dust

    NASA Astrophysics Data System (ADS)

    Wegscheider, S.; Steinlechner, S.; Leuchtenmüller, M.

    2017-02-01

    Industrial wastes such as slags, dust, or precipitation residues contain significant amounts of valuable metals like zinc, lead, and copper as well as precious metals like silver and indium. Nevertheless, a lot of these waste materials are not recycled, and therefore, many valuable metals end up being sent to landfills. Because of harmful components in the waste, it is often necessary to send it to specialized landfills for hazardous wastes, which leads to environmental problems as well as additional costs. Consequently, the recovery of the valuable metals from the residues represents a sensible task to decrease the negative impact on the environment and to reduce costs for maintaining a landfill. In addition, recycling helps to decrease the dependency from primary resources. The present study deals with the behavior of different metals in a pyro-metallurgical treatment for a mixture of jarosite and electric arc furnace dust with a special focus on indium and silver.

  6. Experimental evaluation of high performance base course and road base asphalt concrete with electric arc furnace steel slags.

    PubMed

    Pasetto, Marco; Baldo, Nicola

    2010-09-15

    The paper presents the results of a laboratory study aimed at verifying the use of two types of electric arc furnace (EAF) steel slags as substitutes for natural aggregates, in the composition of base course and road base asphalt concrete (BBAC) for flexible pavements. The trial was composed of a preliminary study of the chemical, physical, mechanical and leaching properties of the EAF steel slags, followed by the mix design and performance characterization of the bituminous mixes, through gyratory compaction tests, permanent deformation tests, stiffness modulus tests at various temperatures, fatigue tests and indirect tensile strength tests. All the mixtures with EAF slags presented better mechanical characteristics than those of the corresponding asphalts with natural aggregate and satisfied the requisites for acceptance in the Italian road sector technical standards, thus resulting as suitable for use in road construction.

  7. The influence of the structure of the metal load removal from liquid steel in electric arc furnaces

    NASA Astrophysics Data System (ADS)

    Pǎcurar, Cristina; Hepuť, Teodor; Crisan, Eugen

    2016-06-01

    One of the main technical and economic indicators in the steel industry and steel respectively the development it is the removal of liquid steel. This indicator depends on several factors, namely technology: the structure and the quality metal load, the degree of preparedness of it, and the content of non-metallic material accompanying the unit of drawing up, the technology for the elaboration, etc. research has been taken into account in drawing up steel electric arc furnace type spring EBT (Electric Bottom taping), seeking to load and removing components of liquid steel. Metal load has been composed of eight metal grades, in some cases with great differences in terms of quality. Data obtained were processed in the EXCEL spreadsheet programs and MATLAB, the results obtained being presented both graphically and analytically. On the basis of the results obtained may opt for a load optimal structure metal.

  8. Investigation of stabilization/solidification for treatment of electric arc furnace dust: Dynamic leaching of monolithic specimens

    SciTech Connect

    Laforest, Guylaine Duchesne, Josee

    2007-12-15

    Diffusion-controlled leaching of heavy metals (Cr, Ni, Pb and Zn) from electric arc furnace dust treated with ground granulated blast furnace slag (GGBFS) and with ordinary Portland cement (OPC) was evaluated. Monolithic specimens were evaluated under dynamic leaching conditions for 84 days with periodic leachant renewal. The influence of leaching time, nature of the leachant, binder type and the water/solid ratio of the monoliths were investigated. Results obtained showed both binders can immobilize heavy metals in the monoliths under dynamic leaching conditions, with cumulative quantity of leached metal under 0.138 mg (Cr). Alkaline leachant increased metal release from specimens and reducing the water/solid ratio of the monolith allowed for a decrease in the cumulative mass of metals leached. Chemical and mineralogical characterizations indicated that the metals were evenly distributed throughout the specimens for both binders. Decalcification was observed on the OPC monolith border following leaching. This decrease in Ca corresponded to an altered zone (20 {mu}m), identified by scanning electron microscopy. The GGBFS sample did not show an altered zone.

  9. Direct determination of silicon in powdered aluminium oxide by use of slurry sampling with in situ fusion graphite-furnace atomic-absorption spectrometry.

    PubMed

    Minami, H; Yoshida, T; Okutsu, K; Zhang, Q; Inoue, S; Atsuya, I

    2001-08-01

    A direct method for determination of silicon in powdered high-purity aluminium oxide samples, by slurry sampling with in situ fusion graphite-furnace atomic-absorption spectrometry (GF-AAS), has been established. A slurry sample was prepared by 10-min ultrasonication of a powdered sample in an aqueous solution containing both sodium carbonate and boric acid as a mixed flux. An appropriate portion of the slurry was introduced into a pyrolytic graphite furnace equipped with a platform. Silicon compounds to be determined and aluminium oxide were fused by the in situ fusion process with the flux in the furnace under optimized heating conditions, and the silicon absorbance was then measured directly. The calibration curve was prepared by use of a silicon standard solution containing the same concentration of the flux as the slurry sample. The accuracy of the proposed method was confirmed by analysis of certified reference materials. The proposed method gave statistically accurate values at the 95% confidence level. The detection limit was 3.3 microg g(-1) in solid samples, when 300 mg/20 mL slurry was prepared and a 10 microL portion of the slurry was measured. The precision of the determination (RSD for more than four separate determinations) was 14% and 2%, respectively, for levels of 10 and 100 microg g(-1) silicon in aluminium oxide.

  10. Flame and graphite furnace atomic absorption spectrometry for trace element determination in vegetable oils, margarine and butter after sample emulsification.

    PubMed

    Ieggli, C V S; Bohrer, D; Do Nascimento, P C; De Carvalho, L M

    2011-05-01

    Trace element analysis plays an important role in oil characterisation and in the detection of oil adulteration because the quality of edible oils and fats is affected by their trace metal content. In this study, the quantification of selected metals in various oils and fats (rice oil, canola oil, sunflower oil, corn oil, soy oil, olive oil, light margarine, regular margarine and butter) was carried out using flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after sample emulsification. FAAS was used to determine the Na, K, Ca, Mg, Zn and Fe levels in the samples, while GFAAS was used for quantifying Cr, Ni, As, Pb, Cd, Cu and Mn, as these elements appeared in the samples at much lower concentrations. Tween-80 and Triton X-100 were employed as surfactants, and emulsions were prepared by a conventional method that involved heating and mixing of the constituents. Complete stabilisation was achieved through magnetic stirring for 15 min at room temperature. The evaluated figures of merit were linearity, accuracy and sensitivity, which were determined by the characteristic concentration and mass. Analysis of spiked samples demonstrated accuracy, which ranged from 90% (Na) to 112% (Fe) for FAAS and from 83% (Cd) to 121% (Pb) for GFAAS measurements. Atomic absorption spectrometry proved to be a promising approach for the analysis of metals in emulsified edible oils and fats. Additionally, under appropriate emulsification conditions (formulation, stirring time and temperature), the emulsions were homogeneous, had excellent stability, and had appropriate viscosity. The proposed method has proved to be simple, sensitive, reproducible, and economical.

  11. Cloud point extraction combined with graphite furnace atomic absorption spectrometry for speciation of Cr(III) in human serum samples.

    PubMed

    Sun, Mei; Wu, Qianghua

    2012-02-23

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace chromium speciation in human serum samples prior to determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. In this method, Cr(III) reacts with 1-(2-pyridylazo)-2-naphthol (PAN) yielding a hydrophobic complex, which is then entrapped in the surfactant-rich phase, whereas Cr(VI) remained in aqueous phase. Thus, separation of Cr(III) and Cr(VI) could be realized. Total chromium was determined after the reduction of Cr(VI) to Cr(III) by using ascorbic acid as reducing reagent. PAN was used not only as chelating reagent in CPE, but also as chemical modifier in GFAAS. Triton X-114 non-ionic surfactant had been used as an extraction medium. The main factors affecting CPE 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 83.5 was obtained for the preconcentration of Cr(III) with 10 mL solution. Under the optimal conditions, the detection limit of Cr(III) was 0.02 μg L⁻¹. The relative standard deviation was 2.6% for intra-day assay precision (n=7, c=10 ng mL⁻¹), values of recovery for chromium were from 92.0% to 94.7% for three samples. This method is simple, accurate, and sensitive and can be applied to determine ultra-trace chromium speciation in human serum. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    PubMed

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

    2013-10-01

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

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

    PubMed

    Filik, Hayati; Cengel, Tayfun; Apak, Reşat

    2009-09-30

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

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

    NASA Astrophysics Data System (ADS)

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

    2017-07-01

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

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

    PubMed Central

    Cai, Jing; Jia, Jinghui; Zhang, Yuzeng; Dong, Weihong

    2017-01-01

    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. PMID:28123908

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

    NASA Astrophysics Data System (ADS)

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

    2008-08-01

    The determination of Mn in diesel, gasoline and naphtha samples at µg L - 1 level by graphite furnace atomic absorption spectrometry, after sample stabilization in a three-component medium (microemulsion) was investigated. Microemulsions were prepared by mixing appropriate volumes of sample, propan-1-ol and nitric acid aqueous solution, and a stable system was immediately and spontaneously formed. After multivariate optimization by central composite design the optimum microemulsion composition as well as the temperature program was defined. In this way, calibration using aqueous analytical solution was possible, since the same sensitivity was observed in the optimized microemulsion media and 0.2% v/v HNO 3. The use of modifier was not necessary. Recoveries at the 3 µg L - 1 level using both inorganic and organic Mn standards spiked solutions ranged from 98 to 107% and the limits of detection were 0.6, 0.5 and 0.3 µg L - 1 in the original diesel, gasoline and naphtha samples, respectively. The Mn characteristic mass 3.4 pg. Typical relative standard deviation ( n = 5) of 8, 6 and 7% were found for the samples prepared as microemulsions at concentration levels of 1.3, 0.8, and 1.5 µg L - 1 , respectively. The total determination cycle lasted 4 min for diesel and 3 min for gasoline and naphtha, equivalent to a sample throughput of 7 h - 1 for duplicate determinations in diesel and 10 h - 1 for duplicate determinations in gasoline and naphtha. Accuracy was also assessed by using other method of analysis (ASTM D 3831-90). No statistically significant differences were found between the results obtained with the proposed method and the reference method in the analysis of real samples.

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

    NASA Astrophysics Data System (ADS)

    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.

  18. Driven Motion and Instability of an Atmospheric Pressure Arc

    SciTech Connect

    Max Karasik

    1999-12-01

    Atmospheric pressure arcs are used extensively in applications such as welding and metallurgy. However, comparatively little is known of the physics of such arcs in external magnetic fields and the mechanisms of the instabilities present. In order to address questions of equilibrium and stability of such arcs, an experimental arc furnace is constructed and operated in air with graphite cathode and steel anode at currents 100-250 A. The arc is diagnosed with a gated intensified camera and a collimated photodiode array, as well as fast voltage and current probes.

  19. Molecular characterization and profile identifications of vanadyl compounds in heavy crude petroleums by liquid chromatography/graphite furnace atomic absorption spectrometry

    SciTech Connect

    Fish, R.H.; Komlenic, J.J.

    1984-03-01

    Four heavy crude petroleums, Boscan, Cerro Negro, Wilmington, and Prudhoe Bay, have been examined by high-performance liquid chromatography in combination with graphite furnace atomic absorption detection (HPLC/GFAA) to provide both a vanadium fingerprint and a molecular weight categorization of the vanadyl porphyrin and non-porphyrin compounds present. We have also attempted to speciate the vanadyl porphyrin and non-porphyrin compounds in these heavy crude oils by comparison of their size exclusion and polar aminocyano separated vanadium histograms to authentic compounds. 35 references, 8 figures, 3 tables.

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

    PubMed

    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).

  1. Direct determination of cadmium and copper in seawater using a transversely heated graphite furnace atomic absorption spectrometer with Zeeman-effect background corrector.

    PubMed

    Chan, M S; Huang, S D

    2000-02-07

    Methods for the direct determination of copper and cadmium in seawater were described using a graphite furnace atomic absorption spectrometer (GFAAS) equipped with a transversely heated graphite atomizer (THGA) and a longitudinal Zeeman effect background corrector. Ammonium nitrate was used as the chemical modifier to determine copper. The mixture of di-ammonium hydrogen phosphate and ammonium nitrate was used as the chemical modifier to determine cadmium. The matrix interference was removed completely so that a simple calibration curve method could be applied. This work is the first one with the capability of determining cadmium in unpolluted seawater directly with GFAAS using calibration curve based on simple aqueous standards. The accuracy of the methods was confirmed by analysis of three kinds of certified reference saline waters. The detection limits (LODs), with injection of a 20-mul aliquot of seawater sample, were 0.06 mug l(-1) for copper and 0.005 mug l(-1) for cadmium.

  2. Surface properties of plasma-functionalized graphite-encapsulated gold nanoparticles prepared by a direct current arc discharge method

    NASA Astrophysics Data System (ADS)

    Yang, Enbo; Chou, Han; Tsumura, Shun; Nagatsu, Masaaki

    2016-05-01

    The graphite-encapsulated gold nanoparticles (Au@C NPs) fabricated by a direct current arc discharge method were surface-functionalized by an inductively-coupled radio frequency ammonia plasma with a particle explosion technique for enhancing surface modification efficiency. To investigate the structural and surface properties of Au@C NPs, characterizations using x-ray diffraction, high resolution transmission electron microscopy and x-ray photoelectron spectroscopy have been conducted on the untreated and plasma treated Au@C NPs. Based on the experimental results, we give insight into the possible formation of Au ions in the interface between the graphite layers and gold core particles of the Au@C NPs. Finally, the role of the plasma treatment on the surface functionalization of Au@C NPs with amino groups is discussed.

  3. Emissions of polychlorinated dibenzo-p-dioxins and dibenzofurans from stack gases of electric arc furnaces and secondary aluminum smelters.

    PubMed

    Lee, Wei-Shan; Chang-Chien, Guo-Ping; Wang, Lin-Chi; Lee, Wen-Jhy; Wu, Kuen-Yuh; Tsai, Perng-Jy

    2005-02-01

    This study investigates the emissions of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) from four electric arc furnaces (EAFs) and eight secondary aluminum smelters (secondary ALSs) in Taiwan. The mean PCDD/F International-Toxicity Equivalents (I-TEQ) concentrations in the stack gases of these EAFs and secondary ALSs are 0.28 ng I-TEQ/Nm3 (relative standard deviation [RSD]= 100%) and 3.3 ng I-TEQ/Nm3 (RSD = 260%), respectively. The high RSDs, especially for those obtained from secondary ALSs, could be caused by the intrinsic differences in their involved feeding materials, furnace operating conditions, and air pollution control devices. The mean I-TEQ emission factor of PCDD/Fs for EAFs (1.8 microg I-TEQ/tonne-feedstock) is lower than that for secondary ALSs (37 microg I-TEQ/tonne-feedstock). This result might be because the involved furnace temperatures for secondary ALSs (650-750 degrees C) are lower than those for EAFs (1600-1700 degrees C), resulting in the deterioration of the combustion condition, leading to the formation of PCDD/Fs during the industrial process. This study found that the total PCDD/F emissions from EAFs (20 g I-TEQ/yr) and secondary ALSs (18 g I-TEQ/yr) are approximately 27, 53, and approximately 24, 49 times higher than those from municipal solid waste incinerators (MSWIs; 0.74 g I-TEQ/yr) and medical waste incinerators (MWIs; 0.37 g I-TEQ/yr), respectively; while those are 44 and 40% of total PCDD/F emission from sinter plants (45 g I-TEQ/ yr), respectively. Considering a more stringent emission limit has been applied to waste incinerators (0.1 ng I-TEQ/Nm3) in Taiwan lately, the results suggest that the control of the emissions from metallurgical processes has become the most important issue for reducing the total PCDD/F emission from industrial sectors to the ambient environment.

  4. Dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometry: ultra trace determination of cadmium in water samples.

    PubMed

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

    2007-03-07

    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 microL methanol (disperser solvent) containing 34 microL 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 microL). Then a 20 microL 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

  5. XPS and XRD study of FeCl3-graphite intercalation compounds prepared by arc discharge in aqueous solution.

    PubMed

    Yan, Zhang; Zhuxia, Zhang; Tianbao, Li; Xuguang, Liu; Bingshe, Xu

    2008-10-01

    A novel one-step synthesis method of FeCl3-graphite intercalation compounds (FeCl3-GICs) by an arc discharge in aqueous solution was reported for the first time. It presented a simply and controllable way to synthesize FeCl3-GICs. The structure of the stage 7 GICs was examined and characterized by X-ray diffraction. X-ray photoelectron spectroscopic study of stage 7 of FeCl3-GICs was also carried out. The change in the binding energy suggests the nature of charge transfer and lowering of Fermi level as has been reported previously for other acceptor intercalation compounds.

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

    PubMed

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

    2016-12-15

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

  7. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of chromium in water by graphite furnace atomic absorption spectrophotometry

    USGS Publications Warehouse

    McLain, B.J.

    1993-01-01

    Graphite furnace atomic absorption spectrophotometry is a sensitive, precise, and accurate method for the determination of chromium in natural water samples. The detection limit for this analytical method is 0.4 microg/L with a working linear limit of 25.0 microg/L. The precision at the detection limit ranges from 20 to 57 percent relative standard deviation (RSD) with an improvement to 4.6 percent RSD for concentrations more than 3 microg/L. Accuracy of this method was determined for a variety of reference standards that was representative of the analytical range. The results were within the established standard deviations. Samples were spiked with known concentrations of chromium with recoveries ranging from 84 to 122 percent. In addition, a comparison of data between graphite furnace atomic absorption spectrophotometry and direct-current plasma atomic emission spectrometry resulted in suitable agreement between the two methods, with an average deviation of +/- 2.0 microg/L throughout the analytical range.

  8. Simultaneous and direct determination of iron and nickel in biological solid samples by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    PubMed

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

    2013-11-15

    The simultaneous and direct determination of nickel and iron in plants and lichens has been investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry. The primary resonance line for nickel at 232.003 nm and the adjacent secondary line for iron at 232.036 nm have been used for this purpose. The optimization of the experimental conditions was performed using a pine needles certified reference material (SRM 1575a). The influence of pyrolysis and atomization temperatures, the amount of solid sample introduced into the graphite furnace and the use of aqueous or solid standard for calibration were studied. The spectral interferences caused by absorption of the concomitants of the solid sample were detected and corrected using a least square algorithm. Aliquots of 0.1-1mg of the solid samples were weighed onto the solid sampling platforms and analyzed directly, without addition of any reagents. The limits of detection were 25 µg kg(-1) for nickel and 0.40 mg kg(-1) for iron and the precision, expressed as the relative standard deviation, ranged from 7% to 12%. The proposed method was used to determine both metals in different bioindicator samples with successful results. © 2013 Elsevier B.V. All rights reserved.

  9. [Characteristics of rubidium forward degenerate four-wave mixing (FDFWM) influenced by the matrix effect of chloride brine in graphite furnace].

    PubMed

    Wang, Jian; Ren, Zhao-Yu; Cheng, Xue-Mei; Miao, Yi-Zhu; Chen, Hao-Wei; Yin, Xun-Li; Wang, Li-Qin; Bai, Jin-Tao

    2012-06-01

    Rb is mainly extracted from brine. The authors studied the matrix effect of chloride brine (NaCl, CaCl2, KCl and MgCl2) on FDFWM (Forward phase-matching degenerate four-wave mixing) of Rb in the graphite furnace. The Rb and other chloride brine concentrations dependences of FDFWM were investigated respectively. The results indicate that with the increase in Rb concentration, FDFWM increases and reaches the highest at 80 ng x mL(-1). With the concentration of Rb sample further increasing, the FDFWM intensity drops. It was also found that when the Rb concentration is low, FDFWM signal is suppressed by the chloride brine, and the suppressing effect gets stronger with the increase in the chloride brine concentration. However, when the Rb concentration is high, FDFWM signal is first enhanced and then suppressed with the increase in the chloride brine concentration. The Cl- interference and Rb ionization in the graphite furnace were employed to explain the experimental results. This work is of important meaning in extracting and analyzing Rb in brine.

  10. Destruction of inorganic municipal solid waste incinerator fly ash in a DC arc plasma furnace.

    PubMed

    Zhao, Peng; Ni, Guohua; Jiang, Yiman; Chen, Longwei; Chen, Mingzhou; Meng, Yuedong

    2010-09-15

    Due to the toxicity of dioxins, furans and heavy metals, there is a growing environmental concern on municipal solid waste incinerator (MSWI) fly ash in China. The purpose of this study is directed towards the volume-reduction of fly ash without any additive by thermal plasma and recycling of vitrified slag. This process uses extremely high-temperature in an oxygen-starved environment to completely decompose complex waste into very simple molecules. For developing the proper plasma processes to treat MSWI fly ash, a new crucible-type plasma furnace was built. The melting process metamorphosed fly ash to granulated slag that was less than 1/3 of the volume of the fly ash, and about 64% of the weight of the fly ash. The safety of the vitrified slag was tested. The properties of the slag were affected by the differences in the cooling methods. Water-cooled and composite-cooled slag showed more excellent resistance against the leaching of heavy metals and can be utilized as building material without toxicity problems. Copyright 2010 Elsevier B.V. All rights reserved.

  11. Removal of hexavalent chromium in carbonic acid solution by oxidizing slag discharged from steelmaking process in electric arc furnace

    NASA Astrophysics Data System (ADS)

    Yokoyama, Seiji; Okazaki, Kohei; Sasano, Junji; Izaki, Masanobu

    2014-02-01

    Hexavalent chromium (Cr(VI)) is well-known to be a strong oxidizer, and is recognized as a carcinogen. Therefore, it is regulated for drinking water, soil, groundwater and sea by the environmental quality standards all over the world. In this study, it was attempted to remove Cr(VI) ion in a carbonic acid solution by the oxidizing slag that was discharged from the normal steelmaking process in an electric arc furnace. After the addition of the slag into the aqueous solution contained Cr(VI) ion, concentrations of Cr(VI) ion and total chromium (Cr(VI) + trivalent chromium (Cr(III)) ions decreased to lower detection limit of them. Therefore, the used slag could reduce Cr(VI) and fix Cr(III) ion on the slag. While Cr(VI) ion existed in the solution, iron did not dissolve from the slag. From the relation between predicted dissolution amount of iron(II) ion and amount of decrease in Cr(VI) ion, the Cr(VI) ion did not react with iron(II) ion dissolved from the slag. Therefore, Cr(VI) ion was removed by the reductive reaction between Cr(VI) ion and the iron(II) oxide (FeO) in the slag. This reaction progressed on the newly appeared surface of iron(II) oxide due to the dissolution of phase composed of calcium etc., which existed around iron(II) oxide grain in the slag.

  12. Aluminum Bronze Alloys to Improve the System Life of Basic Oxygen and Electric Arc Furnace Hoods, Roofs and Side Vents.

    SciTech Connect

    Lawrence C. Boyd Jr.; Dr. Vinod K. Sikka

    2006-12-29

    Energy Industries of Ohio was the lead organization for a consortium that examined the current situation involving the service life of electric arc and basic oxygen furnace hoods, roofs and side vents. Republic Engineered Products (REP), one of the project partners, installed a full-scale Al-Bronze “skirt” in their BOF at their Lorain OH facility, believed to be the first such installation of this alloy in this service. In 24 months of operation, the Al-Bronze skirt has processed a total of 4,563 heats, requiring only 2 shutdowns for maintenance, both related to physical damage to the skirt from operational mishaps. Yearly energy savings related to the REP facility are projected to be ~ 10 billion Btu's with significant additional environmental and productivity benefits. In recognition of the excellent results, this project was selected as the winner of the Ohio’s 2006 Governor’s Award for Excellence in Energy, the state’s award for outstanding achievements in energy efficiency.

  13. Inertization of pyrite cinders and co-inertization with electric arc furnace flue dusts by pyroconsolidation at solid state.

    PubMed

    Viñals, J; Balart, M J; Roca, A

    2002-01-01

    The viability of a pyroconsolidation process to render pyrite cinders inert and to co-inert pyrite cinders with a hazardous polymetallic residue such as electric arc furnace flue dusts (EAF) containing Pb, Cu, Zn, As, Cr, Ni and Mo were investigated. The effects of pyroconsolidation temperature (800-1200 degrees C), milling pyrite cinders and additions of both CaO and EAF on the resulting microstructure of the pellets were determined. The microstructural changes were then compared with the results of the standard leaching tests. Full inertization of pyrite cinders was achieved after milling to < 100 micron followed by a pelletization and pyroconsolidation process at a temperature of 1200 degrees C. This process also allows co-inertization of pyrite cinders with controlled additions of EAF (up to approximately to 10%). Following pyroconsolidation at 1200 degrees C, the metallic elements were inert components in the four main phases: traces of Cr in hematite; Cr, Cu, Zn and Ni in spinel-phase; traces of Cr and Zn in calcium ferrites; and Pb and traces of Cu, Zn and Ba in K-Ca-Al-Fe glassy silicate.

  14. Citotoxicity status of electroplating wastewater prior/after neutralization/purification with alkaline solid residue of electric arc furnace dust.

    PubMed

    Orescanin, Visnja; Kopjar, Nevenka; Durgo, Ksenija; Elez, Loris; Gustek, Stefica Findri; Colic, Jasna Franekic

    2009-02-15

    Toxicological safety of new procedure for the neutralisation/purification of wastewater originated from zinc plating facility was investigated. Wastewater was treated with alkaline solid residue-by-product of zinc recovery from electric arc furnace dust. For determination of cytotoxic potential of untreated and purified wastewater MTT test on HEp2 (human laryngeal carcinoma) and HeLa (human cervical carcinoma) cells lines and alkaline comet assay on human leukocytes were used. Then 100% of the sample as well as different dilutions were tested. Compared to negative control 100, 75 and 50% of the sample of untreated wastewater significantly decreased survival of both HEp2 and HeLa cell lines. In the presence of undiluted sample survival percentage of HeLa and HEp2 cells were only 2.3 and 0.3% respectively. Only undiluted purified wastewater showed slight but insignificant decrease of the survival of both cell lines. Even 0.5% of the sample of original electroplating wastewater exhibited significantly higher value of all comet assay parameters compared to negative control. There was no significant difference between negative control and purified wastewater for any of comet assay parameters. Significantly lower level of primary DNA damage recorded after treatment with purified water, even comparable with negative control, confirmed effectiveness of the purification process.

  15. Distribution of air and serum PCDD/F levels of electric arc furnaces and secondary aluminum and copper smelters.

    PubMed

    Lee, Ching-Chang; Shih, Tung-Seng; Chen, Hsiu-Ling

    2009-12-30

    Metallurgical processes, such as smelting, can generate organic impurities such as organic chloride chemicals, polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans (PCDD/Fs). The objective of this study was to elucidate the serum PCDD/F levels of 134 workers and ambient air levels around electric arc furnaces (EAF), secondary copper smelters and secondary aluminum smelters (ALSs) in Taiwan. The highest serum PCDD/F levels were found in the ALSs workers (21.9 pg WHO-TEQ/g lipid), with lower levels in copper smelter workers (21.5 pg WHO-TEQ/g lipid), and the lowest in the EAF plant workers (18.8 pg WHO-TEQ/g lipid). This was still higher than the levels for residents living within 5 km of municipal waste incinerators (14.0 pg WHO-TEQ/g lipid). For ambient samples, the highest ambient air PCDD/F level was in the copper smelters (12.4 pg WHO-TEQ/Nm(3)), with lower levels in ALSs (7.2 pg WHO-TEQ/Nm(3)), and the lowest in the EAF industry (1.8 pg WHO-TEQ/Nm(3)). The congener profiles were consistent in serum and in air samples collected in the copper smelters, but not for ALSs and EAF. In secondary copper smelters, the air PCDD/Fs levels might be directly linked to the PCDD/Fs accumulated in the workers due to the exceedingly stable congener pattern of the PCDD/F emission.

  16. Removal of vapour phase PCDD/Fs in electric arc furnace steelmaking emissions by sorption using plastics.

    PubMed

    Ooi, Tze Chean; Ewan, Bruce C R; Cliffe, Keith R; Anderson, David R; Fisher, Raymond; Thompson, Dennis

    2008-08-01

    Plastics are potentially suitable for the removal of vapour phase PCDD/Fs in emissions from the electric arc furnace (EAF) steelmaking process. Three different commercial plastics, i.e. polypropylene BE170MO (Borealis A/S, Denmark), polypropylene in the form of 5 mm spheres (The Precision Plastic Ball Co. Ltd., UK) and polyethylene LD605BA (ExxonMobil Chemical, Belgium), have been studied using a novel experimental apparatus for the removal of vapour phase PCDD/Fs. Polypropylene BE170MO was identified to be the most suitable product amongst the three plastics in terms of PCDD/F sorption and potential industrial application. The optimum temperature for PCDD/F sorption on polypropylene BE170MO was below 90 degrees C for a removal efficiency of >99% at an average vapour phase PCDD/F concentration of 3.5 ng I-TEQ/Nm(3). At 130 degrees C, 53% of the PCDD/Fs trapped on polypropylene BE170MO were desorbed.

  17. Hydrometallurgical process for zinc recovery from electric arc furnace dust (EAFD). Part II: Downstream processing and zinc recovery by electrowinning.

    PubMed

    Tsakiridis, P E; Oustadakis, P; Katsiapi, A; Agatzini-Leonardou, S

    2010-07-15

    The characterization and the agitation leaching of electric arc furnace dust (EAFD) by diluted sulphuric acid have been studied in Part I, as a separate article. The aim of the present research work (Part II) is the development of a purification process of the leach liquor for the recovery of high-purity zinc by electrowinning. The proposed hydrometallurgical process consists of the following four (4) unit operations: (1) Removal of iron as easily filterable crystalline basic sulphate salt of the jarosite type, at atmospheric pressure, by chemical precipitation at pH: 3.5 and 95 degrees C. (2) Zinc solvent extraction by Cyanex 272 at pH: 3.5, T: 40 degrees C, with 25% extractant concentration. (3) Stripping of the loaded organic phase by zinc spent electrolyte (62.5 g/L Zn(2+)) at T: 40 degrees C with diluted H(2)SO(4) (3 mol/L). (4) Zinc electrowinning from sulphate solutions (at 38 degrees C) using Al as cathode and Pb as anode. The acidity of the electrolyte was fixed at 180 g/L H(2)SO(4), while the current density was kept constant at 500 A/m(2).

  18. Application of alkaline solid residue of electric arc furnace dust for neutralization/purification of electroplating wastewaters.

    PubMed

    Elez, Loris; Orescanin, Visnja; Sofilic, Tahir; Mikulic, Nenad; Ruk, Damir

    2008-10-01

    The purpose of this work was development of an appropriate procedure for the neutralization/purification of electroplating wastewater (EWW) with alkaline solid residue (ASR) by-product of the alkaline extraction of zinc and lead from electric arc furnace dust (EAFD). Removal efficiency of ASR at optimum purification conditions (pH 8 and mixing time; 20 minutes) for the elements Pb, Cr (VI), Cr (III), Fe, Ni, Cu and Zn were 94.92%, 97.58%, 99.59%, 99.48%, 97.25% and 99.97%, respectively. The concentrations of all elements in the purified wastewater were significantly lower in relation to the upper permissible limit for wastewaters suitable for discharge into the environment. The remaining waste mud was regenerated in the strong alkaline medium and successfully applied once again for the neutralization/purification of EWW. Removal efficiencies of heavy metals accomplished with regenerated waste mud were comparable to these achieved by original ASR. Elemental concentrations in the leachates of the waste mud were in accordance with regulated values.

  19. Radioactively contaminated electric arc furnace dust as an addition to the immobilization mortar in low- and medium-activity repositories.

    PubMed

    Castellote, Marta; Menéndez, Esperanza; Andrade, Carmen; Zuloaga, Pablo; Navarro, Mariano; Ordóñez, Manuel

    2004-05-15

    Electric arc furnace dust (EAFD), generated by the steel-making industry, is in itself an intrinsic hazardous waste; however, the case may also be that scrap used in the process is accidentally contaminated by radioactive elements such as cesium. In this case the resulting EAFD is to be handled as radioactive waste, being duly confined in low- and medium-activity repositories (LMAR). What this paper studies is the reliability of using this radioactive EAFD as an addition in the immobilization mortar of the containers of the LMAR, that is, from the point of view of the durability. Different mixes of mortar containing different percentages of EAFD have been subjected to flexural and compressive strength, initial and final setting time, XRD study, total porosity and pore size distribution, determination of the chloride diffusion coefficient, dimensional stability tests, hydration heat, workability of the fresh mix, and leaching behavior. What is deduced from the results is that for the conditions used in this research, (cement + sand) can be replaced by EAFD upto a ratio [EAFD/(cement + EAFD)] of 46% in the immobilization mortar of LMAR, apparently without any loss in the long-term durability properties of the mortar.

  20. A novel hydrothermal method for zinc extraction and separation from zinc ferrite and electric arc furnace dust

    NASA Astrophysics Data System (ADS)

    Wang, Hui-gang; Li, Yang; Gao, Jian-ming; Zhang, Mei; Guo, Min

    2016-02-01

    A novel hydrothermal process was developed to extract zinc from pure zinc ferrite (ZnFe2O4) nanopowder and zinc-containing electric arc furnace (EAF) dust using hexahydrated ferric chloride (FeCl3·6H2O) as a decomposing agent. The effects of solid FeCl3·6H2O to ZnFe2O4 ratio by mass ( R F/Z), hydrothermal reaction temperature, and time on zinc extraction were systematically investigated. In the results, when the hydrothermal reaction is conducted at 150°C for 2 h with R F/Z of 15:20, the efficiency of zinc extraction from ZnFe2O4 reaches 97.2%, and the concentration of ferric ions (Fe3+) in the leaching solution is nearly zero, indicating a high selectivity for zinc. In addition, the zinc extraction efficiency from the EAF dust reaches 94.5% in the case of the hydrothermal reaction performed at 200°C for 10 h with the solid FeCl3·6H2O to EAF dust ratio by mass ( R F/EAF dust) of 15:10. Zinc and iron separation is achieved by adjusting the pH value of the leaching solution according to the different precipitation pH values of metal hydroxides.

  1. Utilization of Electric Arc Furnace Dust as raw material for the production of ceramic and concrete building products.

    PubMed

    Sikalidis, Constantine; Mitrakas, Manassis

    2006-01-01

    The up to 20 wt% addition of the Electric Arc Furnace Dust (EAFD) hazardous waste on the properties of extruded clay-based ceramic building products fired at various temperatures (850 to 1050 degrees C), as well as of dolomite-concrete products was investigated. Chemical, mineralogical and particle size distribution analyses were performed in order to characterize the used EAFD. The results showed that the ceramic specimens prepared had water absorption, firing shrinkage, apparent density, mechanical strength, colour and leaching behaviour within accepted limits. Addition of 7.5 to 15 wt% EAFD presented improved properties, while 20 wt% seems to be the upper limit. Dolomite-concrete specimens were prepared by vibration and press-forming of mixtures containing cement, sand, dolomite, EAFD and water. Modulus of rupture values were significantly increased by the addition of EAFD. The leaching tests showed stabilization of all toxic metals within the sintered ceramic structure, while the leaching behaviour of lead in dolomite-concrete products needs further detailed study.

  2. Evaluation of ASD systems for electric arc furnace and argon oxygen decarburization refiner baghouse fans. Final report

    SciTech Connect

    1997-11-01

    Adjustable speed drive (ASD) control of the baghouse fans for Electric Arc Furnace (EAF) and Argon Oxygen Decarburization Vessel (AOD) can improve operations, reduce the degree of dust generation, and provide significant energy savings. The purpose of the project was to quantify the benefits, both in energy savings and other process improvements and to demonstrate the methodology of applying adjustable speed drives, to two baghouse fans from a system perspective. The report describes the approach to accomplishing the ASD equipment installation, the test procedure and methodology and provides the test results and economic return. The test results indicated that by using ASDs to control the extraction fan air flow for the EAF and AOD, the following benefits would be achieved on an annual basis: EAF annual energy savings, 267,929 kWh valued at $11,575; EAF dust reduction, overall, 2--3%; EAF dust reduction, during the flatbath period, 35%; and AOD annual energy savings, 1,443,078 kWh valued at $62,341.

  3. Formation of hexachlorobenzene from dusts of an electric arc furnace used in steelmaking: effect of temperature and dust composition.

    PubMed

    Murakami, Taichi; Shimura, Mizuki; Kasai, Eiki

    2008-10-01

    A certain amount of hexachlorobenzene (HCB), designated a persistent organic pollutant (POP) by the Stockholm Convention, is emitted from an electric arc furnace (EAF) used in the steelmaking process. To understand the formation and decomposition behaviors of HCB during the treatment of waste gases from an EAF, characterization of dust samples from EAFs in different plants was conducted. Dusts 1 and 2 were bag filter dusts collected from a common steel plant and a special steel plant, respectively. The initial concentrations of HCB in dusts 1 and 2 were 62 and < 0.1 ng/g of dust, respectively. Then a series of heating experiments was carried out with these dust samples under various conditions. The formation of HCB from both dusts was not significant under an Ar atmosphere, although the amount of formation from dust 1 slightly increased with an increase in the holding temperature. Under an Ar--20% O2 atmosphere, however, a remarkable amount of HCB formed from dust 1 above 573 K. A certain amount of HCB was also formed from dust 2, even though the initial concentration of HCB was very low. Moreover, the coexistence of metallic compounds such as CuCl2 had a significant accelerating effect on the formation of HCB.

  4. Redox speciation analysis of dissolved iron in estuarine and coastal waters with on-line solid phase extraction and graphite furnace atomic absorption spectrometry detection.

    PubMed

    Chen, Yaojin; Feng, Sichao; Huang, Yongming; Yuan, Dongxing

    2015-05-01

    An automatic on-line solid phase extraction (SPE) system employing the flow injection (FI) technique directly coupled to a graphite furnace atomic absorption spectrometer (GFAAS) was established for speciation and determination of dissolved iron in estuarine and coastal waters. Fe(II) was mixed with ferrozine solution in a sample stream to form the Fe(II)-ferrozine complex which was extracted onto a C18 SPE cartridge, eluted with eluent and detected with GFAAS. In a parallel flow channel, Fe(III) was reduced to Fe(II) with ascorbic acid and then detected in the same way as Fe(II). The home-made interface between FI-SPE and GFAAS efficiently realized the sample introduction to the furnace in a semi-automated way. Parameters of the FI-SPE system and graphite furnace program were optimized based on a univariate experimental design and an orthogonal array design. The salinity effect on the method sensitivity was investigated. The proposed method provided a detection limit of 1.38 nmol L(-1) for Fe(II) and 1.87 nmol L(-1) for Fe(II+III). With variation of the sample loading volume, a broadened determination range of 2.5-200 nmol L(-1) iron could be obtained. The proposed method was successfully applied to analyze iron species in samples collected from the Jiulongjiang Estuary, Fujian, China. With the 2-cartridge FI-SPE system developed, on-line simultaneous determination of Fe species with GFAAS was achieved for the first time.

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

    PubMed

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

    2015-01-01

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

  6. Anomalous restoration of graphitic layers from graphene oxide in ethanol environment at ultrahigh temperature using solar furnace

    NASA Astrophysics Data System (ADS)

    Ishida, Takashi; Miyata, Yuichiro; Shinoda, Yoshihiko; Kobayashi, Yoshihiro

    2016-02-01

    The restoration of graphitic structures from defective graphene oxide was examined in a reactive ethanol environment at ultrahigh temperatures. Structural analysis by Raman spectroscopy indicates that turbostratic structures as well as high crystallinity in multilayer graphene were accomplished by an ultrahigh-temperature process in an ethanol environment. This phenomenon is quite anomalous since it is in striking contrast to the results observed in inert environments, where graphitization proceeds significantly to form a Bernal stacking multilayer graphene. The suppression of graphitization in ethanol environments is probably caused by the simultaneous supply of carbon and etching species during the restoration process.

  7. Feasibility of using solid sampling graphite furnace atomic absorption spectrometry for speciation analysis of volatile and non-volatile compounds of nickel and vanadium in crude oil.

    PubMed

    Silva, Márcia M; Damin, Isabel C F; Vale, Maria Goreti R; Welz, Bernhard

    2007-03-30

    A method for the direct determination of volatile and non-volatile nickel and vanadium compounds in crude oil without previous treatment using direct solid sampling graphite furnace atomic absorption spectrometry is proposed. The crude oil samples were weighed directly onto solid sampling platforms using a microbalance and introduced into a transversely heated solid sampling graphite tube. In previous work of our group losses of volatile nickel and vanadium compounds have been detected, whereas other nickel and vanadium compounds were thermally stable up to 1300 and 1600 degrees C, respectively. In order to avoid this problem different chemical modifiers (conventional and permanent) have been investigated. With 400microg of iridium as permanent modifier, the signal started to drop already after two atomization cycles, possibly because of an interaction of nickel (which is a catalyst poison) with iridium. Twenty micrograms of palladium applied in each determination was found to be optimum for both elements. The palladium was deposited on the platform and submitted to a drying step at 150 degrees C for 75s. After that the sample was added onto the platform and submitted to the furnace program. The influence of sample mass on the linearity of the response and on potential measurement errors was also investigated using four samples with different nickel content. For the sample with the lowest nickel concentration the relationship between mass and integrated absorbance was found to be non-linear when a high sample mass was introduced. It was suspected that the modifier had not covered the entire platform surface, which resulted in analyte losses. This problem could be avoided by using 40microL of 0.5g L(-1) Pd with 0.05% Triton X-100. Calibration curves were established with and without modifier, with aqueous standards, oil-in-water emulsions and the certified reference material NIST SRM 1634c (trace metals in residual fuel oil). The sensitivity for aqueous standards

  8. Process stability assessed by selecting Shewhart's psi statistical analysis technique of the influence of matrix modifier and furnace program in the optimization and precision of zinc determinations by graphite furnace atomic absorption spectroscopy.

    PubMed

    Al-Tufail, M; Akram, M; Haq, A

    1999-03-01

    The method previously used in the Toxicology Laboratories of King Faisal Specialist Hospital and Research Center for determining the zinc concentration in serum by Zeeman atomic absorption spectrometer was improved by modifying the matrix modifier and by changing the heated graphite furnace atomization (HGA) program. After trying several methods we failed to achieve the required precision and the accuracy of methods for serum zinc determination. We changed the matrix modifier to a fifty percent mixture (v/v) of 3.90 grams per liter of ammonium phosphate in Type 1 water with 0.2% nitric acid and 1.0 gram per liter of magnesium nitrate in acidic water (0.2% HNO3) with 0.1% triton X-100 was used as matrix modifier. A twenty-five fold dilution of the sample in matrix modifier was injected on the L'vov's platform of the furnace. In order to reduce the high sensitivity of Zn the furnace program was modified. The method is found very robust. The average reproducibility between inter-runs and intra-run is less than 1.59% with a high degree of accuracy. We used two levels of controls i.e. normal or low level and abnormal or high level. The linearity and the detection limit of the assay were 0.9992 and 0.010 micromol/L respectively. Average recovery of the analyte was 98.65%. The X-Bar and R charts were constructed by using Shewhart's statistical analysis technique to assess the test methodology. It was found that the assay is capable and stable for routine clinical and research analysis. The capability index (C(P)) of the assay, an indicator of the precision, was calculated.

  9. Evaluation of electric arc furnace-processed steel slag for dermal corrosion, irritation, and sensitization from dermal contact.

    PubMed

    Suh, Mina; Troese, Matthew J; Hall, Debra A; Yasso, Blair; Yzenas, John J; Proctor, Debora M

    2014-12-01

    Electric arc furnace (EAF) steel slag is alkaline (pH of ~11-12) and contains metals, most notably chromium and nickel, and thus has potential to cause dermal irritation and sensitization at sufficient dose. Dermal contact with EAF slag occurs in many occupational and environmental settings because it is used widely in construction and other industrial sectors for various applications including asphaltic paving, road bases, construction fill, and as feed for cement kilns construction. However, no published study has characterized the potential for dermal effects associated with EAF slag. To assess dermal irritation, corrosion and sensitizing potential of EAF slag, in vitro and in vivo dermal toxicity assays were conducted based on the Organisation for Economic Co-operation and Development (OECD) guidelines. In vitro dermal corrosion and irritation testing (OECD 431 and 439) of EAF slag was conducted using the reconstructed human epidermal (RHE) tissue model. In vivo dermal toxicity and delayed contact sensitization testing (OECD 404 and 406) were conducted in rabbits and guinea pigs, respectively. EAF slag was not corrosive and not irritating in any tests. The results of the delayed contact dermal sensitization test indicate that EAF slag is not a dermal sensitizer. These findings are supported by the observation that metals in EAF slag occur as oxides of low solubility with leachates that are well below toxicity characteristic leaching procedure (TCLP) limits. Based on these results and in accordance to the OECD guidelines, EAF slag is not considered a dermal sensitizer, corrosive or irritant. Copyright © 2014 John Wiley & Sons, Ltd.

  10. Study of The Maximum Uptake Capacity on Various Sizes of Electric Arc Furnace Slag in Phosphorus Aqueous Solutions

    NASA Astrophysics Data System (ADS)

    Afnizan, W. M. W.; Hamdan, R.; Othman, N.

    2016-07-01

    The high content of uncontrolled phosphorus concentration in wastewater has emerged as a major problem recently. The excessive amount of phosphorus that is originated from domestic waste, unproper treated waste from septic tanks, as well as agricultural activities have led to the eutrophication problem. Therefore, a laboratory experiment was initiated to evaluate the potential of the Electric Arc Furnace Slag (EAFS), a by-product waste from steel making industry in removing phosphorus concentrations in aqueous solutions. In this work several particle sizes ranging from (9.5-12.4 mm, 12.5-15.9 mm, 16.0-19.9 mm, 20.0-24.9 mm, 25-37.4 mm) with a known weight (20±0.28 g, 40±0.27 g, 60±0.30 g, 80±0.29 g and 100±0.38 g) were used to study the effect of different particle sizes towards phosphorus removal. Each particle size of EAFS was shaken in synthetic phosphorus solutions (10 mg/l, 20 mg/l, 30 mg/l, 40 mg/l and 50 mg/l) at a contact time of 2 hours. Final concentrations of phosphorus were sampled and the measurement was made using WESTCO Discrete Analyzer equipment. Results showed that the highest of the maximum uptake capacity of each EAFS particle size distribution achieved at 0.287, 0.313, 0.266, 0.241 and 0.25 mg/g as particle size range was varied from 9.5-12.4 mm to 25-37.4 mm. In conclusion, the maximum uptake capacity of each EAFS mostly was determined to occur at adsorbent weight of 20 to 40 g in most conditions.

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

    PubMed

    Anal, Jasha Momo H

    2014-01-01

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

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

    USGS Publications Warehouse

    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.

  13. Influence of experimental parameters on the determination of antimony in seawater by atomic absorption spectrometry using a transversely heated graphite furnace with Zeeman-effect background correction.

    PubMed

    Cabon, Jean Yves

    2002-12-01

    Spectroscopic and electrothermal conditions for the determination of antimony in seawater using a transversely heated graphite furnace with Zeeman-effect background correction have been optimized with the use of an a priori calculation of the detection limit. The lowest limit of detection was obtained with a 2 nm spectral curvatures bandwidth and the use of an electrodeless discharge lamp; however, these experimental conditions resulted in strong premature curvature of calibration curves. Pd(NO(3))(2) can be recommended as a chemical modifier because seawater interference effects are minimized and pretreatment curves up to 1500 degrees C can be used permitting the removal of the major part of the saline matrix before atomization. Under optimized spectroscopic and electrothermal conditions the obtained limit of detection of Sb in seawater was about 0.4 microg L(-1).

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

    PubMed Central

    Anal, Jasha Momo H.

    2014-01-01

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

  15. Lead screening in DBS by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry: application to newborns and pregnant women.

    PubMed

    Rello, Luis; Aramendía, Maite; Belarra, Miguel A; Resano, Martín

    2015-01-01

    DBS have become a clinical specimen especially adequate for establishing home-based collection protocols. In this work, high-resolution continuum source graphite furnace atomic absorption spectrometry is evaluated for the direct monitoring of Pb in DBS, both as a quantitative tool and a screening method. The development of the screening model is based on the establishment of the unreliability region around the threshold limits, 100 or 50 μg l(-1). More than 500 samples were analyzed to validate the model. The screening method demonstrated high sensitivity (the rate of true positives detected was always higher than 95%), an excellent LOD (1 µg l(-1)) and high throughput (10 min per sample).

  16. Graphite furnace and hydride generation atomic absorption spectrometric determination of cadmium, lead, and tin traces in natural surface waters: study of preconcentration technique performance.

    PubMed

    Tsogas, George Z; Giokas, Dimosthenis L; Vlessidis, Athanasios G

    2009-04-30

    In this study three major types of preconcentration methods based upon different principles (cation exchange, physical absorption and hydrophobic extraction) were evaluated and optimized for the extraction and determination of three highly toxic heavy metals namely Cd, Pb and Sn by graphite furnace and hybrid generation atomic absorption spectrometry in real samples. The optimum analytical conditions were examined and the analytical features of each method were revealed and compared. Detection limits as low as 0.003-0.025 microg L(-1) for Cd(2+), 0.05-0.10 microg L(-1) for Pb(2+) and 0.1-0.25 microg L(-1) for Sn(4+) depending on the extraction method were obtained with RSD values between 3.08% and 6.11%. A preliminary assessment of the pollution status of three important natural ecosystems in Epirus region (NW Greece) was performed and some early conclusions were drawn and discussed.

  17. 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

    NASA Astrophysics Data System (ADS)

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

    2005-06-01

    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 °C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 °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.

  18. Antimony in drinking water, red blood cells, and serum: development of analytical methodology using transversely heated graphite furnace atomization-atomic absorption spectrometry.

    PubMed

    Subramanian, K S; Poon, R; Chu, I; Connor, J W

    1997-05-01

    An atomic absorption spectrometric (AAS) method has been developed for determining microg/L levels of Sb in samples of water and blood. The AAS method is based on the concept of stabilized temperature platform furnace atomization (STPF) realized through the use of a transversely heated graphite atomizer (THGA) furnace, longitudinal Zeeman-effect background correction, and matrix modification with palladium nitrate-magnesium nitrate-nitric acid. The method of standard additions is not mandatory. The detection limit (3 standard deviations of the blank) is 2.6 microg Sb/L for the water, red blood cells (RBCs), and serum samples. Data are presented on the degree of accuracy and precision. The THGA-AAS method is simple, fast, and contamination-free because the entire operation from sampling to AAS measurement is carried out in the same tube. The method has been applied to the determination of Sb in some leachate tap water samples derived from a static copper plumbing system containing Sn/Sb solders, and in small samples (0.5 ml) of RBCs and serum derived from rats given Sb-supplemented drinking water.

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

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-11-15

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

  20. 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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

    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 2CO 3 + 4.0% m/v ZnO + 0.1% m/v Triton® X-100 added over the cement sample and heated at 800 °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).

  1. 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

    NASA Astrophysics Data System (ADS)

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

    2007-09-01

    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 °C for 15 min. The surfactant-rich phase was analyzed by GF AAS, employing the optimized pyrolysis temperatures of 900 °C for Pb and 800 °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%.

  2. [A Zeeman graphite furnace atomic absorption spectrometric method for the determination of trace copper and chromium in drinking water].

    PubMed

    Wang, Z

    1999-08-01

    The determination of trace copper and chromium in drinking water is described in this paper using transverse heated graphite atomizer (THGA) with the technique of Zeeman effect background correction without any other matrix modifiers. The method is fast, and simple with low detection limit which makes it possible to be used for routine analysis of drinking water.

  3. Effects of body formulation and firing temperature to properties of ceramic tile incorporated with electric arc furnace (EAF) slag waste

    NASA Astrophysics Data System (ADS)

    Sharif, Nurulakmal Mohd; Lim, Chi Yang; Teo, Pao Ter; Seman, Anasyida Abu

    2017-07-01

    Significant quantities of sludge and slag are generated as waste materials or by-products from steel industries. One of the by-products is Electric Arc Furnace (EAF) steel slag which consists of oxides such as CaO, Al2O3 and FeO. This makes it possible for slag to partially replace the raw materials in ceramic tile production. In our preliminary assessment of incorporating the EAF slag into ceramic tile, it was revealed that at fixed firing temperature of 1150°C, the tile of composition 40 wt.% EAF slag - 60 wt.% ball clay has comparable properties with commercial ceramic tile. Thus, this current study would focus on effects of body formulation (different weight percentages of K-feldspar and silica) and different firing temperatures to properties of EAF slag added ceramic tile. EAF slag from Southern Steel Berhad (SSB) was crushed into micron size (EAF slag content was 40 wt.%) and milled with ball clay, K-feldspar and silica before compacted and fired at 1125°C and 1150°C. The EAF slag added tile was characterized in terms of water absorption, apparent porosity, bulk density, modulus of rupture (MOR) and phase analysis via X-ray diffraction (XRD). The composition of 40 wt.% EAF slag - 30 wt.% ball clay - 10 wt.% K-feldspar - 20 wt.% silica (10F_20S), fired at 1150°C showed the lowest water absorption, apparent porosity and highest bulk density due to enhancement of densification process during firing. However, the same composition of ceramic tile (10F_20S) had the highest MOR at lower firing temperature of 1125°C, contributed by presence of the highest total amount of anorthite and wollastonite reinforcement crystalline phases (78.40 wt.%) in the tile. Overall, both the water absorption and MOR of all ceramic tiles surpassed the requirement regulated by MS ISO 13006:2014 Standard (Annex G: Dry-pressed ceramic tile with low water absorption, Eb ≤ 0.50 % and minimum MOR of 35 MPa).

  4. Hydrometallurgical recovery of zinc and lead from electric arc furnace dust using mononitrilotriacetate anion and hexahydrated ferric chloride.

    PubMed

    Leclerc, Nathalie; Meux, Eric; Lecuire, Jean Marie

    2002-04-26

    The purpose of this work was to study the feasibility at laboratory-scale of a new hydrometallurgical process for treating electric arc furnace dusts (EAFD). The proposed process is intended to extract zinc and lead from EAFD without destroying the iron oxides matrix. So, this material can be recycled by the steel industry. Independently of the origin of the samples, major mineralogical forms present in these wastes are Fe3O4, ZnO, ZnFe2O4 and PbOHCl. The proposed process consists of a hydrometallurgical treatment of wastes based on selective leaching of zinc and lead. Initially, a leaching is carried out utilizing a chelating agent, nitrilotriacetate anion (NTA3-), as the protonated form HNTA2-. Treatment of five EAFD samples for an hour at room temperature with a molar solution of reagent results in total leaching of the ZnO. In all cases the solubilized iron does not exceed 3 wt.%. The recovery of zinc and lead is performed by precipitation of metallic sulfides with a solution of Na2S4 sodium tetrasulfide 2M. These metallic sulfides can be used as metallurgical raw materials and the chelating reagent can be reused in the process after pH adjustment. The results of the normalized leaching test AFNOR X31-210 conducted on the leaching residues, shows that all the samples meet acceptance thresholds for hazardous wastes landfill. However, the residues contain a considerable amount of zinc as ZnFe2O4. The extraction of the zinc element requires the destruction of the ferrite structure. In this process, ZnFe2O4 is treated by FeCl3.6H2O. The reaction consists in a particle O2-/Cl- exchange allowing the recovery of zinc as ZnCl2 and iron as hematite Fe2O3. The separation of these products is accomplished by simple aqueous leaching. All of the zinc is extracted in a 8h treatment at 150 degrees C with a molar ratio FeCl3.6H2O/ZnFe2O4 equal to 10. Ultimate solid residues, which have been concentrated in iron, can be oriented towards the steel industry.

  5. Test Plan: Phase 1 demonstration of 3-phase electric arc melting furnace technology for vitrifying high-sodium content low-level radioactive liquid wastes

    SciTech Connect

    Eaton, W.C.

    1995-05-31

    This document provides a test plan for the conduct of electric arc vitrification testing by a vendor in support of the Hanford Tank Waste Remediation System (TWRS) Low-Level Waste (LLW) Vitrification Program. The vendor providing this test plan and conducting the work detailed within it [one of seven selected for glass melter testing under Purchase Order MMI-SVV-384216] is the US Bureau of Mines, Department of the Interior, Albany Research Center, Albany, Oregon. This test plan is for Phase I activities described in the above Purchase Order. Test conduct includes feed preparation activities and melting of glass with Hanford LLW Double-Shell Slurry Feed waste simulant in a 3-phase electric arc (carbon electrode) furnace.

  6. A combined arc-melting and tilt-casting furnace for the manufacture of high-purity bulk metallic glass materials.

    PubMed

    Soinila, E; Pihlajamäki, T; Bossuyt, S; Hänninen, H

    2011-07-01

    An arc-melting furnace which includes a tilt-casting facility was designed and built, for the purpose of producing bulk metallic glass specimens. Tilt-casting was chosen because reportedly, in combination with high-purity processing, it produces the best fatigue endurance in Zr-based bulk metallic glasses. Incorporating the alloying and casting facilities in a single piece of equipment reduces the amount of laboratory space and capital investment needed. Eliminating the sample transfer step from the production process also saves time and reduces sample contamination. This is important because the glass forming ability in many alloy systems, such as Zr-based glass-forming alloys, deteriorates rapidly with increasing oxygen content of the specimen. The challenge was to create a versatile instrument, in which high purity conditions can be maintained throughout the process, even when melting alloys with high affinity for oxygen. Therefore, the design provides a high-vacuum chamber to be filled with a low-oxygen inert atmosphere, and takes special care to keep the system hermetically sealed throughout the process. In particular, movements of the arc-melting electrode and sample manipulator arm are accommodated by deformable metal bellows, rather than sliding O-ring seals, and the whole furnace is tilted for tilt-casting. This performance of the furnace is demonstrated by alloying and casting Zr(55)Cu(30)Al(10)Ni(5) directly into rods up to ø 10 mm which are verified to be amorphous by x-ray diffraction and differential scanning calorimetry, and to exhibit locally ductile fracture at liquid nitrogen temperature.

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

    PubMed

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

    2017-10-03

    In addition to beneficial health effects, fluoride can also have adverse effects on humans, animals, and plants if the daily intake is strongly elevated. One main source of fluoride uptake is water, and thus several ordinances exist in Germany that declare permissible concentrations of fluoride in, for example, drinking water, mineral water, and landfill seepage water. Controlling the fluoride concentrations in aqueous matrices necessitate valid and fast analytical methods. In this work an alternative method for the determination of fluoride in surface waters based on high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) was applied. Fluoride detection was made possible by the formation of a diatomic molecule, GaF, and detection of characteristic molecular absorption. On HR-CS-GFMAS parameter optimization, the method was adapted to surface water sample analysis. The influence of potential main matrix constituents such as Na(+), Ca(2+), Mg(2+), and Cl(-) as well as surface water sampling/storage conditions on the molecular absorption signal of GaF was investigated. Method validation demonstrated a low limit of detection (8.1 μg L(-1)) and a low limit of quantification (26.9 μg L(-1)), both sufficient for direct river water sample analysis after 0.45-μm filtration. The optimized HR-CS-GFMAS method was applied for the analysis of real water samples from the rivers Rhine and Moselle. For method validation, samples were also analyzed by an ion chromatography (IC) method. IC and HR-CS-GFMAS results both agreed well. In comparison with IC, HR-CS-GFMAS has higher sample throughput, a lower limit of detection and a lower limit of quantification, and higher selectivity, and is a very suitable method for the analysis of dissolved fluoride in river water. Graphical abstract High-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) was applied for the quantitative analysis of dissolved

  8. Development and validation of a general non-digestive method for the determination of palladium in bulk pharmaceutical chemicals and their synthetic intermediates by graphite furnace atomic absorption spectroscopy.

    PubMed

    Wang, T; Walden, S; Egan, R

    1997-02-01

    A simple, selective, sensitive, accurate and relatively inexpensive method for the determination of palladium in bulk pharmaceutical chemicals (BPC) and their synthetic intermediates by graphite furnace atomic absorption spectroscopy has been developed and validated. Sample preparation by direct dissolution of sample in 70% nitric acid is simple and effective without adverse effects. The limit of detection and the limit of quantitation of the method were determined to be 0.7 ppm and 2 ppm respectively in BPC.

  9. Determination of trace impurities in boron nitride by graphite furnace atomic absorption spectrometry and electrothermal vaporization inductively coupled plasma optical emission spectrometry using solid sampling

    NASA Astrophysics Data System (ADS)

    Barth, P.; Hassler, J.; Kudrik, I.; Krivan, V.

    2007-09-01

    Two digestion-free methods for trace analysis of boron nitride based on graphite furnace atomic absorption spectrometry (GFAAS) and electrothermal vaporization inductively coupled plasma spectrometry optical emission (ETV-ICP-OES) using direct solid sampling have been developed and applied to the determination of Al, Ca, Cr, Cu, Fe, Mg, Mn, Si, Ti and Zr in four boron nitride materials in concentration intervals of 1-23, 54-735, 0.05-21, 0.005-1.3, 1.6-112, 4.5-20, 0.03-1.8, 6-46, 38-170 and 0.4-2.3 μg g - 1 , respectively. At optimized experimental conditions, with both methods, effective in-situ analyte/matrix separation was achieved and calibration could be performed using calibration curves measured with aqueous standard solutions. In solid sampling GFAAS, before sampling, the platform was covered with graphite powder and, for determination of Si, also the Pd/Mg(NO 3) 2 modifier was used. In the determination of all analyte elements by solid sampling ETV-ICP-OES, Freon R12 was added to argon carrier gas. For solid sampling GFAAS and ETV-ICP-OES, the achievable limits of detection were within 5 (Cu)-130 (Si) ng g - 1 and 8 (Cu)-200 (Si) ng g - 1 , respectively. The results obtained by these two methods for four boron nitride materials of different purity grades are compared each with the other and with those obtained in analysis of digests by ICP-OES. The performance of the two solid sampling methods is compared and discussed.

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

    PubMed

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

    2013-11-15

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

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

    PubMed

    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.

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

    PubMed

    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.

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

    PubMed Central

    Mohadesi, Alireza; Falahnejad, Masoumeh

    2012-01-01

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

  14. Determination of Selenium and Arsenic Ions in Edible Mushroom Samples by Novel Chloride-Oxalic Acid Deep Eutectic Solvent Extraction Using Graphite Furnace-Atomic Absorption Spectrometry.

    PubMed

    Zounr, Rizwan Ali; Tuzen, Mustafa; Khuhawar, Muhammad Yar

    2017-08-18

    In present study, we proposed the application of a deep eutectic solvent (DES) made up of choline chloride (ChCl) and oxalic acid (Ox) for the dissolution of different edible mushroom samples for the determination of selenium (Se) and arsenic (As) ions. Therefore, an innovative, green, novel, and inexpensive method based on ChCl–Ox as the DES was developed for the determination of Se and As ions in mushroom species by graphite furnace-atomic absorption spectrometry. The important analytical parameters were also optimized. The LODs for Se and As ions were found to be 0.32 and 0.50 µg/L, respectively. The LOQs for Se and As ions were found to be 1.06 and 1.65 µg/L, respectively. The RSD was observed to be less than 5% for both analyte ions. The accuracy of the developed method was confirmed by analyzing mushroom powder Certified Reference Material CS-M-3 (Boletus edulis). The developed technique was effectively useful for the determination of Se and As ions in different species of mushroom samples from Turkey.

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

    PubMed

    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.

  16. Determination of Pb and Cd in Garlic Herb (Allium sativum) Planted in Gilan and Khuzestan Provinces Using Graphite Furnace Atomic Absorption Spectrometry

    PubMed Central

    Ramezani, Zahra; Aghel, Nasrin; Amirabedin, Negar

    2012-01-01

    Background Foods are enriched with variety of chemical elements. Some of these elements are necessary for human health. These elements enter in liquid, the cells and other organs, certain amount of these elements are essential for body organs to work properly. Objectives This research was conducted to compare the level of lead and cadmium contamination in garlic species planted in Ramhormoz and Rasht and discuss about the source of this contaminations. Materials and Methods Twenty composite samples were collected from each province, Khozestan (Ramhormoz) and Gilan (Rasht). Each sample was burned according to instruction reported in AOAC. Then the white residue was dissolved in diluted nitric acid then the Pb and Cd contents were determined using graphite furnace atomic absorption spectrometer at 217 and 228.8 nm, respectively. No Pb level was detected in garlic cultured in both cities. The mean concentration of cadmium was 0.40 and 0.58 mg/kg in garlics planted in Ramhormoz and Rasht, respectively. Results Statistical analysis showed significant difference between mean concentration of cadmium in Rasht garlic and the permitted value (P < 0.001). The cadmium level in Rasht garlic is much higher than the standard level. Conclusions In order to test the reliability of the data obtained using this method, randomly selected samples were spiked with Pb and Cd standard solutions. The cadmium and lead recovery were reported 93.93 and 90.18 percent. PMID:24624152

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

    NASA Astrophysics Data System (ADS)

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

    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- 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.

  18. Determination of lead in medicinal plants by high-resolution continuum source graphite furnace atomic absorption spectrometry using direct solid sampling.

    PubMed

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

    2012-10-15

    A procedure is proposed for Pb determination in medicinal plants by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) using direct solid sampling. Among Pd(NO(3))(2), Pd/Mg(NO(3))(2), NH(4)H(2)PO(4) and the W-coated platform tested as chemical modifiers, Pd(NO(3))(2) presented the best performance. Calibration plots (10-1000 pg Pb) with regression coefficients better than 0.999 were typically obtained. Accuracy was checked for Pb determination in five plant certified reference materials. Results were in agreement with reference values at a 95% confidence level (paired t-test). Medicinal plant samples were analyzed by the proposed procedure and line-source GF AAS using slurry sampling as a comparative technique. The RSD was 10% (n=3) for a sample containing 0.88 μg g(-1) Pb. The limit of quantification (dry mass) was 0.024 μg g(-1). The contents of Pb in medicinal plant samples varied in the 0.30-1.94 μg g(-1) range.

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

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2017-04-01

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

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

    PubMed

    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.

  2. Ionic liquid-based extraction followed by graphite-furnace atomic absorption spectrometry for the determination of trace heavy metals in high-purity iron metal.

    PubMed

    Matsumiya, Hiroaki; Kato, Tatsuya; Hiraide, Masataka

    2014-02-01

    The analysis of high-purity materials for trace impurities is an important and challenging task. The present paper describes a facile and sensitive method for the determination of trace heavy metals in high-purity iron metal. Trace heavy metals in an iron sample solution were rapidly and selectively preconcentrated by the extraction into a tiny volume of an ionic liquid [1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide] for the determination by graphite-furnace atomic absorption spectrometry (GFAAS). A nitrogen-donating neutral ligand, 2,4,6-tris(2-pyridyl)-1,3,5-triazine (TPTZ), was found to be effective in the ionic liquid-based selective extraction, allowing the nearly complete (~99.8%) elimination of the iron matrix. The combination with the optimized GFAAS was successful. The detectability reached sub-μg g(-1) levels in iron metal. The novel use of TPTZ in ionic liquid-based extraction followed by GFAAS was successfully applied to the determination of traces of Co, Ni, Cu, Cd, and Pb in certified reference materials for high-purity iron metal.

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

    PubMed

    Krawczyk, Magdalena

    2014-01-01

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

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2017-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    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 °C and 2400 °C, respectively. Slopes of calibration curves (50-750 pg Cr, R2 > 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.

  7. Determination of sulfur in crude oil using high-resolution continuum source molecular absorption spectrometry of the SnS molecule in a graphite furnace.

    PubMed

    Cadorim, Heloisa R; Pereira, Éderson R; Carasek, Eduardo; Welz, Bernhard; de Andrade, Jailson B

    2016-01-01

    An analytical method for the determination of sulfur, as the tin mono-sulfide (SnS) molecule, in crude oil using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) has been developed. The molecular absorbance of the SnS has been measured using the wavelength at 271.624 nm and the crude oil samples were prepared as micro-emulsions due to their high viscosity. Several chemical modifiers (Ir, Pd, Ru, Zr) were tested and palladium was chosen, because it exhibited the best performance. The heating program was optimized by comparing the pyrolysis and vaporization curves obtained for an aqueous sulfur standard and a micro-emulsion of a crude oil certified reference material (CRM). The optimum pyrolysis and vaporization temperatures were found to be 600 and 2000°C, respectively. The limit of detection and the characteristic mass using micro-emulsion analysis of crude oil samples were 5.8 and 13.3 ng S. Accuracy and precision of the method has been evaluated using two crude oil CRM (NIST 2721 and NIST 2722), showing good agreement with the informed or certified values.

  8. Study of the versatility of a graphite furnace atomic absorption spectrometric method for the determination of cadmium in the environmental field.

    PubMed

    Rucandio, M Isabel; Petit-Domínguez, M Dolores

    2002-01-01

    Cadmium is a representative example of trace elements that are insidious and widespread health hazards. In contemporary environmental analysis, there is a clear trend toward its determination over a wide range of concentrations in complex matrixes. This paper describes a versatile method for the determination of Cd at various levels (0.1-500 microg/g) in several sample types, such as soils, sediments, coals, ashes, sewage sludges, animal tissues, and plants, by graphite furnace atomic absorption spectrometry with Zeeman background correction. The effect of the individual presence of about 50 elements, with an interference/analyte concentration ratio of up to 10(5), was tested; recoveries of Cd ranged from 93 to 106%. The influence of different media, such as HNO3, HCI, HF, H2SO4, HClO4, acetic acid, hydroxylammonium chloride, and ammonium acetate, in several concentrations, was also tested. From these studies it can be concluded that the analytical procedure is scarcely matrix dependent, and the results obtained for a wide diversity of reference materials are in good agreement with the certified values.

  9. A novel assay of cell rubidium uptake using graphite furnace atomic absorption: application to rats on a magnesium-deficient diet.

    PubMed

    Zhen, Yueying; Franz, Kay B; Graves, Steven W

    2005-05-01

    The [Na,K]ATPase or sodium pump (SP) is a ubiquitous membrane cation transport system. Because of its potential participation in the pathophysiology of essential hypertension and cataract formation, the SP is under active investigation to detail its function and control. In this paper, we describe a novel, nonradioactive method of measuring SP ion transport activity in intact red blood cells (RBCs) using graphite furnace atomic absorption measurement of rubidium ion (Rb) uptake. This method provided sensitivity comparable to radioactive techniques, as assessed by experiments with human red blood cells (RBC) and ouabain, a known SP inhibitor, but this analytical approach eliminates the use of radioisotopes common to other Rb uptake assay methods. As a demonstration of its broader utility, the assay was used to assess the effects of dietary magnesium intake on SP-mediated ion transport in the RBCs of diet-controlled rats. Rats on 7 weeks of a magnesium-deficient (MgD) diet showed significant reductions in serum magnesium concentration, although levels remained in the lower region of the reference interval for healthy, magnesium replete animals. Red cell Rb uptake was significantly reduced in cells from the magnesium-restricted animals, demonstrating the sensitivity of Rb uptake to reduced magnesium intake, despite serum levels that fell within the reported normal range, and the utility of this Rb uptake assay in measuring physiological changes in SP function.

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

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2017-06-01

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

  12. Ultrasound-assisted ion-pair dispersive liquid-liquid microextraction of trace amounts of lead in water samples prior to graphite furnace atomic absorption spectrometry determination.

    PubMed

    Afzali, Daryoush; Mohadesi, Ali Reza; Falahnejad, Masoumeh; Bahadori, Behnoosh

    2013-01-01

    A new ion-pair dispersive liquid-liquid microextraction method is described for separation and preconcentration of trace amounts of lead in different water samples. Graphite furnace atomic absorption spectrometry was used for determination of lead. The ion association complex between lead and iodide ions that forms is PbI4(-2)-tetradecyl-dimethylbenzylammonium, which is extracted into fine droplets of chlorobenzene. In order to reach the optimized experimental conditions, the influence of different parameters, such as concentration of KI, nature and volume of extraction solvents, pH effect, extraction time, and the period and speed of sonication and centrifugation, were optimized. The LOD was 0.08 ng/mL and the linear dynamic range was 0.20-8.0 ng/mL in initial solution with a correlation coefficient of 0.9985. Under the optimum conditions, the enrichment factor was 555.5. The proposed method was successfully applied for separation and determination of lead in sea, rain, river, and drinking water samples.

  13. Ultrasound-assisted emulsification microextraction based on solidification floating organic drop trace amounts of manganese prior to graphite furnace atomic absorption spectrometry determination.

    PubMed

    Mohadesi, Alireza; Falahnejad, Masoumeh

    2012-01-01

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

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

    PubMed

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

    2016-04-01

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

  15. 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

    NASA Astrophysics Data System (ADS)

    Araujo, Rennan G. O.; Vignola, Fabíola; Castilho, Ivan N. B.; Borges, Daniel L. G.; Welz, Bernhard; Vale, Maria Goreti R.; Smichowski, Patricia; Ferreira, Sérgio L. C.; Becker-Ross, Helmut

    2011-05-01

    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 (3σ), based on ten atomizations of an unexposed filter, was 40 ng g - 1 , corresponding to 0.12 ng m - 3 in the air for a typical air volume of 1440 m 3 collected within 24 h. The limit of quantification was 150 ng g -1, equivalent to 0.41 ng m -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 -1 and 381 ± 24 ng g -1. These values correspond to a mercury concentration in the air between < 0.12 ng m -3 and 1.47 ± 0.09 ng m -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.

  16. Solidified floating organic drop microextraction (SFODME) for simultaneous separation/preconcentration and determination of cobalt and nickel by graphite furnace atomic absorption spectrometry (GFAAS).

    PubMed

    Bidabadi, Mahboubeh Shirani; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji

    2009-07-15

    Solidified floating organic drop microextraction (SFODME), combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for simultaneous separation/enrichment and determination of trace amounts of nickel and cobalt in surface waters and sea water. 1-(2-Pyridylazo)-2-naphthol (PAN) was used as chelating agent. The main parameters affecting the performance of SFODME, such as pH, concentration of PAN, extraction time, stirring rate, extraction temperature, sample volume and nature of the solvent were optimized. Under the optimum experimental conditions, a good relative standard deviation for six determination of 20 ng l(-1) of Co(II) and Ni(II) were 4.6 and 3.6%, respectively. An enrichment factor of 502 and 497 and detection limits of 0.4 and 0.3 ng l(-1) for cobalt and nickel were obtained, respectively. The procedure was applied to tap water, well water, river water and sea water, and accuracy was assessed through the analysis of certified reference water or recovery experiments.

  17. Lead and cadmium in human placentas and maternal and neonatal blood (in a heavily polluted area) measured by graphite furnace atomic absorption spectrometry.

    PubMed Central

    Baranowska, I

    1995-01-01

    OBJECTIVE--To measure the concentrations of the trace elements lead and cadmium in human placenta and in maternal and neonatal (cord) blood. To assess the influence of the strongly polluted environment on the content of metals in tissues and on the permeability of placenta to cadmium and lead. Various methods of mineralisation were tested before analysis. METHODS--Graphite furnace atomic absorption spectrometry was used for the determination of lead and cadmium. The samples for analysis were prepared by mineralisation under pressure in a Teflon bomb (HNO3, 110 degrees C), by wet ashing under normal pressure (HNO3 + H2O2 for 12 hours), and by microwave digestion in concentrated nitric acid. RESULTS--In analysed samples the following mean concentrations of cadmium and lead were found: in venous blood Pb = 72.50 ng/ml, Cd = 4.90 ng/ml; in placenta Pb = 0.50 microgram/g, Cd = 0.11 microgram/g; in cord blood Pb = 38.31 ng/ml, Cd = 1.13 ng/ml. CONCLUSION--High concentrations of lead and cadmium were found in placentas and in maternal blood whereas in neonatal blood there was an increased concentration of lead and only traces of cadmium. It is concluded that the placenta is a better barrier for cadmium than for lead. Among the examined methods of mineralisation, microwave digestion was the best. PMID:7795737

  18. Selective determination of arsenic (III, V), antimony (III, V), selenium (IV, VI) and tellurium (IV, VI) by extraction and graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Chung, Chan-Huan; Iwamoto, Etsuro; Yamamoto, Manabu; Yamamoto, Yuroku

    Parameters were investigated for the selective determination of arsenic (III, V), antimony (III, V), selenium (IV, VI) and tellurium (IV, VI) by graphite furnace atomic absorption spectrometry combined with extraction using an ammonium pyrrolidinedithiocarbamate and chloroform + carbon tetrachloride solvent mixture. Selenium (VI) and tellurium (VI) were not extracted over the entire range of pH studied, although the extraction conditions for the other species were not critical. It was found that the incorporation of titanium (III) chloride as a reducing agent in the extraction procedure made it possible to differentiate the above elements in the higher and lower oxidation states. The four elements at the low oxidation state were first extracted at pH 5 and after the addition of titanium chloride to the aqueous phase, the species in the high oxidation state were extracted at about pH 0.3. High sensitivity for the determination of the eight species was obtained. Interferences by many foreign ions have been studied.

  19. [Selenium determination in plasma/serum by inductively coupled plasma mass spectrometry (ICP-MS): comparison with graphite furnace atomic absorption spectrometry (GF-AAS)].

    PubMed

    Janasik, Beata; Trzcinka-Ochocka, Małgorzata; Brodzka, Renata

    2011-01-01

    The present study was aimed at comparing two techniques of selenium (Se) determination in serum/plasma samples: inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption (GF-AAS). Blood samples were collected by venipuncture, using Venosafe closed blood sampling system. The samples were centrifuged. The measurements were performed by Elan DRC-e mass spectrometry, Perkin Elmer, SCIEX, USA and Unicam Solar 989 QZ atomic absorption spectrometry. Reference material, Clincheck Serum Control Level 1 (Recipe, Germany), was used to verify the determinations. The Laboratory participates in external quality control (G-EQUAS). Analytical parameters for both techniques are respectively: ICP-MS--precision 5.9%, limit of detection 0.19 microg/l, repeatability 5.5%, trueness 2.4%, bias 97.6%, GF-AAS--precision 8%, limit of detection 3.4 microg/l, repeatability 7.2%, trueness 6.8%, bias 93.2%. The benefits of the ICP-MS technique are high accuracy, low detection limits and the possibility of multi-element analysis.

  20. Determination of trace lead in water samples by graphite furnace atomic absorption spectrometry after preconcentration with nanometer titanium dioxide immobilized on silica gel.

    PubMed

    Liu, Rui; Liang, Pei

    2008-03-21

    Nanometer titanium dioxide immobilized on silica gel (immobilized nanometer TiO2) was prepared by sol-gel method and characterized using X-ray diffraction (XRD) and scanning electron microscope (SEM). The adsorptive capability of immobilized nanometer TiO2 for lead was assessed in this work using column method. It was found that lead can be quantitatively retained by immobilized nanometer TiO2 in the pH range 4-7, then eluted completely with 1.0molL(-1) HCl. The adsorption capacity of immobilized nanometer TiO2 for Pb was found to be 3.16mgg(-1). A new method has been developed for the determination of trace lead based on preconcentration with a microcolumn packed with immobilized nanometer TiO2 prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS). The detection limit of this method for Pb was 9.5ngL(-1) with an enrichment factor of 50, and the relative standard deviations (R.S.D.s) was 3.2% at the 10ngmL(-1) Pb level. The method was validated using a certified reference material, and was applied for the determination of trace lead in water samples.

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

    NASA Astrophysics Data System (ADS)

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

    2014-06-01

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

  2. Determination of chromium(VI) and lead(II) in drinking water by electrokinetic flow analysis system and graphite furnace atomic absorption spectrometry.

    PubMed

    Yang, L; He, Y Z; Gan, W E; Li, M; Qu, Q S; Lin, X Q

    2001-08-30

    An electrokinetic flow analysis system (EKFA) using an electroosmotic pump (Peo) and a bi-directional electrostacking (BDES) unit is introduced in this paper. Large flow range, moderate carrier pressure, low performance voltage and stable flow rate, especially in mulmin(-1) level, are the main specialties of the Peo. Diethanolamine, 0.5 mM, is selected as its carrier to improve the pump efficiency and stability further. Moreover, BDES, a feasibility investigation for the simultaneous separation and pre-concentration of cations and anions, and graphite furnace atomic absorption spectrometry (GFAAS) determination are presented. The calibration series for both of Cr(VI) and Pb(II) are from 0.2 to 40 mugl(-1) with 10 mul pipette volume and GFAAS determination directly. The detection limit of Cr(VI) and Pb(II) with 10 min BDES is 10 and 13 ngl(-1)(3sigma of blank, n=11), respectively. The recovery of Cr(VI) and Pb(II) is (103-105)+/-1% and (95.9-96.9)+/-1.0% with three independent determinations, respectively. The investigated method is also suitable for the simultaneous separation and pre-concentration of trace cations and anions in low conductivity sample solutions with different detection instruments.

  3. [Direct determination of lead and cadmium in soil by slurry-sampling graphite furnace atomic absorption spectrometry using matrix modification technique].

    PubMed

    Sun, Han-Wen; Wen, Xiao-Hua; Liang, Shu-Xuan

    2006-05-01

    A method for the direct determination of lead and cadmium in soil by slurry-sampling graphite furnace-atomic absorption spectrometry using NH4 H2 PO4 as matrix modifier was developed. The effects of slurry stability, particle size of sample, matrix modifiers, ashing temperature, atomization temperature and common coexistent components on the signal intensities of lead and cadmium were investigated. The apparent activation energies of lead and cadmium were measured based on the linear relationship between the logarithm value of atomization peak time and atomization temperature. The mechanism of matrix modification was discussed. Under optimized conditions, the detection limit was 9.05 x 10(-10) g x mL(-1) for Pb and 1.76 x 10(-11) g x mL(-1) for Cd. The recoveries were in the range of 91%-97% for Pb and 93%-109% for Cd. The relative standard deviations were in the range of 4.2%-7.8%.

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

    NASA Astrophysics Data System (ADS)

    Kamyabi, Mohammad Ali; Aghaei, Ali

    2017-02-01

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

  5. The study of applicability of dithiocarbamate-coated fullerene C 60 for preconcentration of palladium for graphite furnace atomic absorption spectrometric determination in environmental samples

    NASA Astrophysics Data System (ADS)

    Leśniewska, Barbara A.; Godlewska, Iwona; Godlewska—Żyłkiewicz, Beata

    2005-03-01

    The present method comprises an off-line enrichment of Pd on the fullerene, C 60, coated with ammonium pyrrolidinedithiocarbamate (APDC), followed by the elution of formed Pd-chelate with ethanol and the subsequent determination of Pd from the eluate by graphite furnace atomic absorption spectrometry. By using fullerene loaded with 0.1% APDC, the analytical system is simplified as the sample can be directly preconcentrated on the column. The following parameters affecting the preconcentration of Pd on C 60 were optimized: amount of ligand used for the coating of fullerene, sample pH, kind of eluent, sample and eluent flow rates, volume and number of fractions of eluent used. The sorption efficiency for Pd on coated fullerene was 99.2±1.1%. The best elution efficiency for Pd from the column was obtained with 0.6 ml of ethanol at a flow rate of 0.2 ml min -1. The limit of detection was 0.044 ng ml -1. The effect of sample pretreatment procedure on the preconcentration of Pd by evaluated method is discussed. The content of Pd in road dust (179.2±17.4 ng g -1) determined by proposed method was in agreement with the results obtained with a reference method. The low recovery of analyte (64%) was obtained for geological material CRM SARM-7 (platinum ore) due to the much higher concentration of interfering elements.

  6. Determination of trace aluminum in biological and water samples by cloud point extraction preconcentration and graphite furnace atomic absorption spectrometry detection.

    PubMed

    Sang, Hongbo; Liang, Pei; Du, Dan

    2008-06-15

    A cloud point extraction (CPE) method for the preconcentration of trace aluminum prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) has been developed. The CPE method is based on the complex of Al(III) with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP), and then entrapped in non-ionic surfactant Triton X-114. PMBP was used not only as chelating reagent in CPE preconcentration, but also as chemical modifier in GFAAS determination. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of PMBP and Triton X-114, equilibration temperature and time, were investigated in detail. An enrichment factor of 37 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of this method for Al(III) is 0.09 ng mL(-1), and the relative standard deviation is 4.7% at 10 ng mL(-1) Al(III) level (n=7). The proposed method has been applied for determination of trace amount of aluminum in biological and water samples with satisfactory results.

  7. Development of rapid slurry methods for flame and direct current plasma emission and graphite furnace atomic absorption analysis of solid animal tissue

    SciTech Connect

    Fietkau, R.

    1986-01-01

    Studies are presented describing developments in the rapid, direct atomic spectrochemical analysis of meat samples by the technique of slurry atomization. The number of elements that can be determined in meat slurry samples has been increased and the concentration range that can be detected extended to included analysis at the part per billion as well as the percent level. Slurry atomization involves the rapid preparation procedure whereby the sample is simple homogenized with deionized distilled water prior to analysis. In this manner, rapid, quantitative analysis of hot dogs (processed meat) for dietary salt (Na, K) was achieved by premixed air-natural gas flame emission spectrometry. Quantitative analysis of mechanically separated meat for residual bone fragments (as Ca) was attained using a simple photometer when the premixed air-acetylene flame was used. The phosphate interference of the Ca emission signal was overcome by placing an insert in the spray chamber which decreased the droplet size of the aerosol reaching the flame. Slight matrix modification in the form of 2% nitric acid was necessary to solubilize the Ca from the bone fragments. Determining elements present at very low concentrations i.e. part per billion levels, in homogenized beef liver was evaluated using graphite furnace atomic absorption and shown to be viable for determinations of Pb, Cd, Cr, and Ni. Qualitative multielement analysis of several types of meat slurries by direct current plasma (DCP) emission spectrometry using both photographic and electronic modes of detection was reported for the first time.

  8. Multivariate approach in the optimization procedures for the direct determination of manganese in serum samples by graphite furnace atomic absorption spectrometry.

    PubMed

    Fabrino, Henrique José Ferraz; Silveira, Josianne Nicácio; Neto, Waldomiro Borges; Goes, Alfredo Miranda; Beinner, Mark Anthony; da Silva, José Bento Borba

    2011-10-01

    A method for direct determination of manganese (Mn) in human serum by graphite furnace atomic absorption spectrometry (GFAAS) was proposed in this work. The samples were only diluted 1:4 with nitric acid 1% (v/v) and Triton(®) X-100 0.1% (v/v). The optimization of the instrumental conditions was made using multivariate approach. A factorial design (2(3)) was employed to investigate the tendency of the most intense absorbance signal. The pyrolysis and atomization temperatures and the use of modifier were available and only the parameter modifier use did not have a significant effect on the response. A Center Composed Design (CCD) presented best temperatures of 430 °C and 2568 °C for pyrolysis and atomization, respectively. The method allowed the determination of manganese with a curve varying from 0.7 to 3.3 μg/L. Recovery studies in three concentration levels (n=7 for each level) presented results from 98 ± 5 to 102 ± 7 %. The detection limit was 0.2 μg/L, the quantifying limit was 0.7 μg/L, and the characteristic mass, 1.3 ± 0.2 pg. Intra- and interassay studies showed coefficients of variation of 4.7-7.0% (n=21) and 6-8%(n=63), respectively. The method was applied for the determination of manganese in 53 samples obtaining concentrations from 3.9 to 13.7 μg/L.

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

    NASA Astrophysics Data System (ADS)

    Huber, Charles S.; Vale, Maria Goreti R.; Welz, Bernhard; Andrade, Jailson B.; Dessuy, Morgana B.

    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- 1 and 4.7 mg kg- 1, respectively.

  10. Automatic microemulsion preparation for metals determination in fuel samples using a flow-batch analyzer and graphite furnace atomic absorption spectrometry.

    PubMed

    Cunha, Francisco Antônio S; Sousa, Rafael A; Harding, David P; Cadore, Solange; Almeida, Luciano F; Araújo, Mário César U

    2012-05-21

    The principal thermodynamic advantages of using microemulsions over standard emulsions for flow metal analysis are the greatly increased analyte stability and emulsive homogeneity that improve both the ease of sample preparation, and the analytical result. In this study a piston propelled flow-batch analyzer (PFBA) for the determination of Cu, Cr and Pb in gasoline and naphtha by graphite furnace atomic absorption spectrometry (GF AAS) was explored. Investigative phase modeling for low dilution was conducted both for gasoline and naphtha microemulsions. Rheological considerations were also explored including a mathematical flow derivation to fine tune the system's operational parameters, and the GF AAS coupling. Both manual and automated procedures for microemulsion preparation were compared. The results of the paired t test at a 95% confidence level showed no significant differences between them. Further recovery test results confirmed a negligible matrix effect of the sample on the analyte absorption signals and an efficient stabilization of the samples (with metals) submitted to microemulsion treatment. The accuracy of the developed procedure was attested by good recovery percentages in the ranges of 100.0±3.5% for Pb in the naphtha samples, and 100.2±3.4% and 100.7±4.6% for Cu and Cr, respectively in gasoline samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Determination of cadmium in coal using solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry.

    PubMed

    da Silva, Alessandra Furtado; Borges, Daniel L G; Lepri, Fábio Grandis; Welz, Bernhard; Curtius, Adilson J; Heitmann, Uwe

    2005-08-01

    This work describes the development of a method to determine cadmium in coal, in which iridium is used as a permanent chemical modifier and calibration is performed against aqueous standards by high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). This new instrumental concept makes the whole spectral environment in the vicinity of the analytical line accessible, providing a lot more data than just the change in absorbance over time available from conventional instruments. The application of Ir (400 microg) as a permanent chemical modifier, thermally deposited on the pyrolytic graphite platform surface, allowed pyrolysis temperatures of 700 degrees C to be used, which was sufficiently high to significantly reduce the continuous background that occurred before the analyte signal at pyrolysis temperatures <700 degrees C. Structured background absorption also occurred after the analyte signal when atomization temperatures of >1600 degrees C were used, which arose from the electron-excitation spectrum (with rotational fine structure) of a diatomic molecule. Under optimized conditions (pyrolysis at 700 degrees C and atomization at 1500 degrees C), interference-free determination of cadmium in seven certified coal reference materials and two real samples was achieved by direct solid sampling and calibrating against aqueous standards, resulting in good agreement with the certified values (where available) at the 95% confidence level. A characteristic mass of 0.4 pg and a detection limit of 2 ng g(-1), calculated for a sample mass of 1.0 mg coal, was obtained. A precision (expressed as the relative standard deviation, RSD) of <10% was typically obtained when coal samples in the mass range 0.6-1.2 mg were analyzed.

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

    NASA Astrophysics Data System (ADS)

    Becker, Emilene; Rampazzo, Roger T.; Dessuy, Morgana B.; Vale, Maria Goreti R.; da Silva, Márcia M.; Welz, Bernhard; Katskov, Dmitri A.

    2011-05-01

    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 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 μg L -1, respectively, for THPA, and 1.8 and 5.9 μg L -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 μg L -1 in the samples analyzed in this work.

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

    NASA Astrophysics Data System (ADS)

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

    2011-05-01

    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.

  14. Determination of iodine via the spectrum of barium mono-iodide using high-resolution continuum source molecular absorption spectrometry in a graphite furnace

    NASA Astrophysics Data System (ADS)

    Huang, Mao Dong; Becker-Ross, Helmut; Florek, Stefan; Okruss, Michael; Welz, Bernhard; Morés, Silvane

    2009-07-01

    Molecular absorption spectra of the diatomic molecules AlI, GaI, InI, TlI, MgI, CaI, SrI and BaI, generated in a graphite furnace, were studied using a high-resolution echelle spectrometer with the aim of finding a simple, reliable and sensitive analytical method for the determination of iodine. Among them, the barium mono-iodide (BaI) was found to have the strongest absorption bands around 538 nm and 560 nm, each of them consisting of a series of well-resolved rotational lines with half-widths of about 40-50 pm. The strongest BaI line, the band head at 538.308 nm has been evaluated systematically for its analytical use for the determination of iodine. High concentrations of hydrochloric acid (or chloride), hydrofluoric acid (or fluoride), iron, potassium and sodium resulted in significant reduction of the BaI molecular absorption. Apart from this, no other serious spectral or non-spectral interference has been observed. Different chemical forms of iodine, such as iodide, iodate and organically bound iodine produced identical BaI absorption sensitivity. The detection limit for iodine was 600 pg, and the calibration curve was linear up to 250 ng iodine. Two real samples with different chemical forms of iodine were analyzed using the proposed method. One sample was an iodide pill with a specified iodide content of 200 mg, the other one was a thyroid hormone pill with a specified content of 63.5 mg. The results were in good or satisfactory agreement with those of independent methods, the potentiometric titration and the inductively coupled plasma time-of-flight mass spectrometry (ICP-ToF-MS); the deviations were 2% and 8% for the iodide and the thyroid hormone sample, respectively. The relative standard deviation of the analytical results ( n = 3) was below 2%.

  15. Determination of the in vivo pharmacokinetics of palladium-bacteriopheophorbide (WST09) in EMT6 tumour-bearing Balb/c mice using graphite furnace atomic absorption spectroscopy.

    PubMed

    Brun, Pierre Hervé; DeGroot, Jennifer L; Dickson, Eva F Gudgin; Farahani, Mohsen; Pottier, Roy H

    2004-01-01

    Palladium-bacteriopheophorbide (WST09), a novel bacteriochlorophyll derivative, is currently being investigated for use as a photodynamic therapy (PDT) drug due to its strong absorption in the near-infrared region and its ability to efficiently generate singlet oxygen when irradiated. In this study, we determined the pharmacokinetics and tissue distribution of WST09 in female EMT6 tumour-bearing Balb/c mice in order to determine if selective accumulation of this drug occurs in tumour tissue. A total of 41 mice were administered WST09 by bolus injection into the tail vein at a dose level of 5.0 +/- 0.8 mg kg(-1). Three to six mice were sacrificed at each of 0.08, 0.25, 0.5, 1.0, 3.0, 6.0, 9.0, 12, 24, 48, 72, and 96 h post injection, and an additional three control mice were sacrificed without having been administered WST09. Terminal blood samples as well as liver, skin, muscle, kidney and tumour samples were obtained from each mouse and analyzed for palladium content (from WST09) using graphite furnace atomic absorption spectroscopy (GFAAS). The representative concentration of WST09 in the plasma and tissues was then calculated. Biphasic kinetics were observed in the plasma, kidney, and liver with clearance from each of these tissues being relatively rapid. Skin, muscle and tumour did not show any significant accumulation at all time points investigated. No selective drug accumulation was seen in the tumour and normal tissues, relative to plasma. Thus the results of this study indicate that vascular targeting resulting from WST09 in the circulation, as opposed to selective WST09 accumulation in tumour tissues, may be responsible for PDT effects in tumours that have been observed in other WST09 studies.

  16. Determination of zinc in serum, blood, and ultrafiltrate fluid from patients on hemofiltration by graphite furnace/atomic absorption spectroscopy or flow injection analysis/atomic absorption spectroscopy.

    PubMed

    de Blas, O J; Rodriguez, R S; Mendez, J H; Tomero, J A; Gomez, B de L; Gonzalez, S V

    1994-01-01

    Two methods were optimized for the determination of zinc in samples of blood, serum, and ultrafiltrate fluid from patients with chronic renal impairment undergoing hemofiltration. In the first procedure, after acid digestion of the samples, Zn in blood and serum is determined by a system coupled to flow injection analysis and atomic absorption spectroscopy. The method is rapid, automated, simple, needs small amounts of sample, and has acceptable analytical characteristics. The analytical characteristics obtained were as follows: determination range of method, 0.05-2.0 ppm of Zn; precision as coefficient of variation (CV), 5.3%; recovery, 95-105%; and detection limit (DL), 0.02 ppm. The second method is optimized for ultrafiltrate fluid because the sensitivity of the first procedure is not suitable for the levels of Zn (ppb or ng/mL) in these samples. The technique chosen was atomic absorption spectroscopy with electrothermal atomization in a graphite furnace. The analytical characteristics obtained were as follows: determination range of method, 0.3-2.0 ppb Zn; CV, 5.7%; recovery, 93-107%; and DL, 0.12 ppb. The methods were used to determine zinc in samples of blood, serum, and ultrafiltrate fluid from 5 patients with chronic renal impairment undergoing hemofiltration to discover whether there were significant differences in the zinc contents of blood, serum, and ultrafiltrate fluid after the hemofiltration process. An analysis of variance of the experimental data obtained from a randomly selected group of 5 patients showed that zinc concentrations in the ultrafiltrate fluid, venous blood, and venous serum do not vary during hemofiltration (p < 0.05), whereas in arterial blood and serum, the time factor has a significant effect.

  17. Simultaneous determination of iron and nickel in fluoropolymers by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry.

    PubMed

    Soares, Bruno M; Santos, Rafael F; Bolzan, Rodrigo C; Muller, Edson I; Primel, Ednei G; Duarte, Fabio A

    2016-11-01

    This paper reports the development of a method of simultaneous determination of iron and nickel in fluoropolymers by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with direct solid sampling. In order to carry out simultaneous measurements, both the main resonance line of nickel (232.003nm) and the adjacent secondary line of iron (232.036nm) were monitored in the same spectral window. The proposed method was optimized with a perfluoroalkoxy (PFA) sample and was applied to the determination of iron and nickel in fluorinated ethylene propylene (FEP) and modified polytetrafluoroethylene (PTFE-TFM) samples. Pyrolysis and atomization temperatures, as well as the use of Pd and H2 (during pyrolysis) as chemical modifiers, were carefully investigated. Compromise temperatures for pyrolysis and atomization of both analytes were achieved at 800 and 2300°C, respectively, using only 0.5Lmin(-1) H2 as chemical modifier during pyrolysis. Calibration curves were performed with aqueous standards by using a single solution which contained both analytes. Limits of detection were 221 and 9.6ngg(-1) for iron and nickel, respectively. Analyte concentrations in all samples ranged from 3.53 to 12.4µgg(-1) for iron and from 37 to 78ngg(-1) for nickel, with relative standard deviation less than 19%. Accuracy was evaluated by comparing these results with those obtained by inductively coupled plasma mass spectrometry after sample digestion by microwave-induced combustion and no significant statistical difference was observed.

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

    PubMed

    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.

  19. Determination of chlorine via the CaCl molecule by high-resolution continuum source graphite furnace molecular absorption spectrometry and direct solid sample analysis.

    PubMed

    Guarda, Ananda; Aramendía, Maite; Andrés, Irene; García-Ruiz, Esperanza; do Nascimento, Paulo Cícero; Resano, Martín

    2017-01-01

    This work investigates the possibilities of high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of Cl in solid samples via the CaCl molecule and measurement of its molecular absorption. The method proposed is based on addition of 400µg Ca as molecule-forming reagent and of 20µgPd as chemical modifier, which helps to stabilize the analyte and enhances sensitivity. The molecular spectrum for CaCl offers different lines with different limits of detection and linear ranges, which permitted to analyze solid samples with different Cl contents. The lowest limit of detection (0.75ng Cl, corresponding to 0.75µgg(-1) for a typical sample mass of 1mg) could be achieved by combination of three of the most sensitive lines in the vicinity of 620.862nm, while the amplest linear range (up to 860ng Cl) was achieved by selection of the less sensitive line at 377.501nm. The method developed enabled the direct determination of Cl in solid samples using simple external calibration with aqueous standards. Good precision (5-9% RSD) and accuracy was attained in a series of certified samples of very different nature (i.e. coal, iron oxide, polyethylene, human hair, pine needles, rice flour and milk) and with very different Cl contents, ranging from about 50µgg(-1) to 1% (w/w) Cl. The method appears as particularly useful for Cl determination in samples with elevated Ca contents, for which biased results with other diatomic molecules, such as AlCl or SrCl, may be obtained.

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

    PubMed

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

    2015-03-01

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

  1. Direct and simultaneous determination of Cr and Fe in crude oil using high-resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Dittert, Ingrid M.; Silva, Jessee S. A.; Araujo, Rennan G. O.; Curtius, Adilson J.; Welz, Bernhard; Becker-Ross, Helmut

    2009-06-01

    A simple, fast and sensitive direct method for the simultaneous determination of Cr and Fe in crude oil samples is proposed using high-resolution continuum source graphite furnace atomic absorption spectrometry. No sample preparation is used except for a 10-minute homogenization in an ultrasonic bath. Aliquots of 0.1-4 mg of the samples are weighed onto solid sampling platforms and analyzed directly using aqueous standards for calibration. The simultaneous determination was possible because there is a secondary Fe line at 358.120 nm in the vicinity of the most sensitive Cr line at 357.868 nm, and both absorption lines were within the wavelength interval covered by the linear charge-coupled device array detector. It has also been of advantage that the sensitivity ratio between the two analytical lines corresponded roughly to the concentration ratio of the two elements found in crude oil, and that both analytes have very similar volatility, so that no compromises had to be made regarding pyrolysis and atomization temperatures. Two oil reference materials have been analyzed and the results were in agreement with the certified or reported values. Characteristic masses of 3.6 pg and 0.5 ng were obtained for Cr and Fe, respectively. The limits of detection (3 σ, n = 10) were 1 µg kg - 1 for Cr and 0.6 mg kg - 1 for Fe, and the precision, expressed as the relative standard deviation, ranged from 4 to 20%, which is often acceptable for a rapid direct analytical procedure. Five crude oils samples were analyzed.

  2. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of low-level silver by graphite furnace atomic absorption spectrophotometry

    USGS Publications Warehouse

    Damrau, D.L.

    1993-01-01

    Increased awareness of the quality of water in the United States has led to the development of a method for determining low levels (0.2-5.0 microg/L) of silver in water samples. Use of graphite furnace atomic absorption spectrophotometry provides a sensitive, precise, and accurate method for determining low-level silver in samples of low ionic-strength water, precipitation water, and natural water. The minimum detection limit determined for low-level silver is 0.2 microg/L. Precision data were collected on natural-water samples and SRWS (Standard Reference Water Samples). The overall percent relative standard deviation for natural-water samples with silver concentrations more than 0.2 microg/L was less than 40 percent throughout the analytical range. For the SRWS with concentrations more than 0.2 microg/L, the overall percent relative standard deviation was less than 25 percent throughout the analytical range. The accuracy of the results was determined by spiking 6 natural-water samples with different known concentrations of the silver standard. The recoveries ranged from 61 to 119 percent at the 0.5-microg/L spike level. At the 1.25-microg/L spike level, the recoveries ranged from 92 to 106 percent. For the high spike level at 3.0 microg/L, the recoveries ranged from 65 to 113 percent. The measured concentrations of silver obtained from known samples were within the Branch of Quality Assurance accepted limits of 1 1/2 standard deviations on the basis of the SRWS program for Inter-Laboratory studies.

  3. Investigation of high-resolution absorption spectra of diatomic sulfides of group 14 elements in graphite furnace and the comparison of their performance for sulfur determination

    NASA Astrophysics Data System (ADS)

    Huang, Mao Dong; Becker-Ross, Helmut; Florek, Stefan; Abad, Carlos; Okruss, Michael

    2017-09-01

    For the purpose of finding suitable molecules applicable to sulfur determination and to compare their analytical sensitivity systematically, high-resolution overview molecular absorption spectra of sulfides of group 14 elements produced in a graphite furnace were investigated. To that end a modular simultaneous echelle spectrograph (MOSES) was used, which allows recording sub-ranges of spectra out of a total wavelength range from 190 nm to 735 nm. The combined overview spectra show a complex structure with many vibrational bands, each of them consisting of a multitude of sharp rotational lines. The absorption of rotational lines of SiS (282.910 nm), GeS (295.209 nm), SnS (271.578 nm), and PbS (335.085 nm) has been analyzed for optimizing the particular experimental conditions regarding to the sulfur determination. Using the commercial CS AAS instrument contrAA 600 under optimized conditions such as the temperature program, the modification of the platform with Zr and the use of chemical modifiers, the achieved characteristic masses for sulfur are 12 ng (CS), 15.7 ng (SiS), 9.4 ng (GeS), 20 ng (SnS), and 220 ng (PbS). The first four sulfides provide an analytical sensitivity at roughly the same level, but the GeS molecule seems to be the best one with respect to analytical sensitivity and flexibility in molecular formation control. The PbS molecule provides the lowest analytical sensitivity, and together with its low bond strength it is not recommended for sulfur determination.

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

    PubMed

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

    2016-04-07

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

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

    NASA Astrophysics Data System (ADS)

    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.

  6. 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

    NASA Astrophysics Data System (ADS)

    Borges, Aline R.; Becker, Emilene M.; Dessuy, Morgana B.; Vale, Maria Goreti R.; Welz, Bernhard

    2014-02-01

    In this work, chemical modifiers in solution (Pd/Mg, NH4H2PO4 and NH4NO3/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 NH4H2PO4 was abandoned due to severe spectral interference even at the 283.3-nm line. For Pd/Mg and NH4NO3/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- 1 using Pd/Mg and 29 ng g- 1 using NH4NO3/Pd. Among the permanent modifiers investigated, the LOD was 22 ng g- 1 Pb for Ir and 10 ng g- 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 NH4NO3/Pd.

  7. First order speciation of As using flow injection hydride generation atomic absorption spectrometry with in-situ trapping of the arsine in a graphite furnace

    NASA Astrophysics Data System (ADS)

    Willie, Scott N.

    1996-12-01

    A simple method is described to distinguish between As species that react with sodium tetrahydroborate (III) to form AsH 3 and the naturally occurring As species that are unreactive. Results for this rudimentary or "first order" speciation scheme are reported for biological tissue, aquatic plant material, urine and natural water samples. Biological tissue and aquatic plant samples were briefly solubilized in a mixture of 50% nitric acid, no sample preparation was required for the urine or natural water samples. Organoarsenic species which do not react with sodium borohydride under acidic conditions such as arsenobetaine, arsenocholine and tetramethylarsenic, are converted to As(V) by on-line photo-oxidation or microwave heating in a mixture of 0.5 M NaOH and 0.05 M K 2S 2O 8. The sample is subsequently acidified, reduced with sodium borohydride and the generated arsine is trapped in a heated graphite furnace prior to atomization. The superior detection limit (0.14 ng) of the trapping technique permits the dilution of most types of samples, minimizing or eliminating interference effects. Without photolysis or microwave heating a combined result for As(III), As(V), monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA) is obtained. Results are reported for the first order speciation of As in a suite of certified reference materials (CRMs) including National Research Council (NRC) biological tissues and natural water samples, Community Bureau of Reference (BCR) aquatic plant materials and the National Institute of Standards and Technology (NIST) SRM 267ON urine sample. The determination of a non-hydride forming As fraction in untreated urine and natural water certified reference materials (CRMs) has revealed a species of As previously undetected in NRC seawater CRMs.

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

    PubMed

    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 < 0.01). There was no significant difference between coagulated and uncoagulated samples run by 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.

  9. Sequential determination of Cd and Cr in biomass samples and their ashes using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis.

    PubMed

    Duarte, Alvaro T; Dessuy, Morgana B; Vale, Maria Goreti R; Welz, Bernhard; de Andrade, Jailson B

    2013-10-15

    High-resolution continuum source graphite furnace atomic absorption spectrometry, because of the use of only one radiation source for all elements, offers the possibility of sequential determination of two or more elements from the same sample aliquot if their volatilities are significantly different. Cd and Cr were determined sequentially in samples of biomass and biomass ashes employing direct solid sample analysis. The use of a chemical modifier was found to be not necessary, and calibration could be carried out using aqueous standard solutions. A pyrolysis temperature of 400°C and an atomization temperature of 1500°C were used for the determination of Cd; no losses of Cr were observed at this temperature. After the atomization of Cd the wavelength was changed and Cr atomized at 2600°C. The limits of detection (LOD) and quantification (LOQ) were 1.1 μg kg(-1) and 3.7 μg kg(-1), respectively, for Cd and 21 μg kg(-1) and 70 μg kg(-1), respectively, for Cr using the most sensitive line at 357.869 nm, or 90 μg kg(-1) and 300 μg kg(-1), respectively, using the less sensitive line at 428.972 nm. The precision, expressed as relative standard deviation was around 10%, which is typical for direct solid sample analysis. The values found for Cd in biomass samples were between <1.1 µg kg(-1) and 789 µg kg(-1), whereas those for Cr were between 7.9 mg kg(-1) and 89 mg kg(-1); the values found in the ashes were significantly lower for Cd, between <1.1 µg kg(-1) and 6.3 µg kg(-1), whereas the trend was not so clear for Cr, where the values were between 3.4 mg kg(-1) and 28 mg kg(-1).

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

    NASA Astrophysics Data System (ADS)

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

    2011-05-01

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

  11. A dried urine spot test to simultaneously monitor Mo and Ti levels using solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Rello, L.; Lapeña, A. C.; Aramendía, M.; Belarra, M. A.; Resano, M.

    2013-03-01

    Home-based collection protocols for clinical specimens are actively pursued as a means of improving life quality of patients that require frequent controls, such as patients with metallic prosthesis, for whom monitoring the evolution of Mo and Ti in biological fluids may play a decisive role to detect prosthesis mal-functioning. The collection of biological fluids on clinical filter papers provides a simple way to implement these protocols. This work explores the potential of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for the simultaneous and direct determination of Mo and Ti in urine, after its deposition onto clinical filter paper, giving rise to a dried urine spot. The approach used for depositing the sample was found crucial to develop a quantitative method, since the filter paper acts as a chromatographic support and produces a differential distribution of the target analytes. Furthermore, the high spreading of urine onto a filter paper results in a small amount of urine per surface unit, and thus, ultimately, in lack of sensitivity. In order to circumvent these problems, the use of an alternative approach based on the use of pre-cut 17 × 19 mm filter paper pieces onto which larger amounts of sample (500 μL) can be retained by single deposition was proposed and evaluated. In this way, an approximately 12-fold increase in sensitivity and a more homogeneous distribution of the target analytes were obtained, permitting the development of a quantification strategy based on the use of matrix-matched urine samples of known analyte concentrations, which were subjected to the same procedure as the samples. Accuracy of this method, which provides LODs of 1.5 μg L- 1 for Mo and 6.5 μg L- 1 for Ti, was demonstrated after analysis of urine reference materials. Overall, the performance of the method developed is promising, being likely suitable for determination of other analytes in dried urine spots.

  12. Determination of subnanogram per cubic meter concentrations of metals in the air of a trace metal clean room by impaction graphite furnace atomic absorption and laser excited atomic fluorescence spectrometry.

    PubMed

    Liang, Z W; Wei, G T; Irwin, R L; Walton, A P; Michel, R G; Sneddon, J

    1990-07-15

    Air, drawn by vacuum through a jet, was impacted against the inside surface of an atomic absorption graphite electrothermal atomizer (ETA). The amounts of the particles thus collected were determined at the ng m-3 level by graphite furnace atomic absorption or at the pg m-3 level by laser excited atomic fluorescence. The overall reproducibility of two sets of measurements, made 7 months apart, was 23%, with no significant difference between the two sets of data, based on Student's "t" test at the 95% confidence level. Short-term reproducibility varied from 13% to 34% depending upon the air concentration of the metal. The method shows promise for monitoring long-term effectiveness of the filtering systems in trace metal clean rooms. It was not possible to test for accuracy, due to the low concentrations involved, but accuracy was expected to be within a factor of 2 or 3 of the actual value, based on theoretical aspects of impaction.

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

    PubMed

    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.

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

    PubMed

    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.

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

    PubMed

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

    2015-10-01

    A novel microwave-assisted dispersive liquid-liquid microextraction (MADLLME) technique according to the solidification of a floating organic droplet (SFO) and graphite furnace atomic absorption spectrometry (GFAAS) used for the extraction and determination of lead ions in lipsticks and hair dyes made in different countries. Lipstick and hair dye samples of different brands and colours were collected from local market in Kermanshah, Iran. After sample treatment with microwave-assisted acid digestion, an appropriate mixture of acetone, 1-undecanol and diethyl dithiophosphoric acid was injected rapidly into the aqueous sample containing lead ions, and as a result, cloudy mixture was formed. After centrifugation, the test tube was cooled for few minutes. The solidified 1-undecanol on top of the solution was transferred into a suitable vial and injected into the analytical instrument. Under the optimum experimental conditions (extraction solvent: 30 μL of 1-undecanol; disperser solvent: 500 μL of acetone; ligand concentration: 0.15% (v/v); pH: ~1.5 and without salt added), the enhancement factor of 96 was obtained. The calibration graphs were linear in the range of 0.3-50 μg kg(-1) with a correlation coefficient (r(2) ) more than 0.995. The detection limit was 0.1 μg kg(-1) . Consequently, the developed method was successfully applied to extract and determine lead ions in the lipsticks and hair dyes, and favourable results were obtained. The proposed method which applied in cosmetics showed excellent relative recoveries (90-109.7%) with relative standard deviations <8.3% (n = 3) for all samples. The study revealed that the concentration of lead found in lipsticks and hair dyes on the Kermanshah market is far below the recommended limits as applied in Germany (20 mg kg(-1) ) and Canada (10 mg kg(-1) ) and confirmed that very low levels of lead are technically available in the final cosmetic products. © 2015 Society of Cosmetic Scientists and the Soci

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

    NASA Astrophysics Data System (ADS)

    Jiang, Hongmei; Hu, Bin; Chen, Beibei; Zu, Wanqing

    2008-07-01

    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 - 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 μg L - 1 and 0.4 μg L - 1 (as Hg) with precisions (RSDs (%), c = 5 μg L - 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 - 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 material of NRCC DORM-2 dogfish

  17. Direct determination of Hg in polymers by solid sampling-graphite furnace atomic absorption spectrometry. A comparison of the performance of line source and continuum source instrumentation

    NASA Astrophysics Data System (ADS)

    Resano, M.; Briceño, J.; Belarra, M. A.

    2009-06-01

    This work explores the potential of solid sampling-graphite furnace atomic absorption spectrometry (SS-GFAAS) for the fast and direct determination of Hg in polymers. Eight certified reference materials with different composition (polyethylene-PE-, polystyrene-PS-, poly vinyl chloride-PVC- and acrylonitrile butadiene styrene-ABS-) were selected for the study, covering a wide Hg content range (from 20 to 1100 μg g - 1 ). The difficulties found in achieving a selective atomization of the analyte from these samples were partially mitigated by the maintenance of the Ar flow during the atomization step, leading to an improved signal-to-background ratio. Even then, when a line source (LS) GFAAS instrument was employed for analysis, it was only possible to develop truly accurate procedures relying on the use of aqueous standards for calibration for PE and PVC samples, and different atomization conditions (1200 °C and 1300 °C, respectively) were needed for the two types of samples. The use of high-resolution continuum source (HR-CS) GFAAS instrumentation permitted to improve this situation significantly thanks to its higher potential for the correction of high and fast changing background. With such an instrument, satisfactory results could be obtained for all the samples under study using the same atomization conditions (1200 °C) and aqueous standard solutions for calibration. Additionally, the HR-CS GFAAS technique presented a lower limit of detection (0.6 μg g - 1 for CS and 2.2 μg g - 1 for LS), a broader linear range (10 to 320 Hg ng for CS, and 20 to 200 ng for LS), and a somewhat improved sensitivity (approximately 0.0030 s ng - 1 for CS using the three central pixels for quantification, and approximately 0.0025 s ng - 1 for LS). Overall, the use of HR-CS GFAAS permits obtaining significant advantages for the determination of this complex analyte in plastics, such as straightforward calibration with aqueous standards, a high sample throughput (15 min per

  18. Method development for the determination of cadmium in fertilizer samples using high-resolution continuum source graphite furnace atomic absorption spectrometry and slurry sampling

    NASA Astrophysics Data System (ADS)

    Borges, Aline R.; Becker, Emilene M.; Lequeux, Céline; Vale, Maria Goreti R.; Ferreira, Sergio L. C.; Welz, Bernhard

    2011-07-01

    The determination of cadmium (Cd) in fertilizers is of major interest, as this element can cause growth problems in plants, and also affect animals and humans. High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with charge-coupled device (CCD) array detection overcomes several of the limitations encountered with conventional line source AAS, especially the problem of accurate background measurement and correction. In this work an analytical method has been developed to determine Cd in fertilizer samples by HR-CS GF AAS using slurry sampling. Both a mixture of 10 μg Pd + 6 μg Mg in solution and 400 μg of iridium as permanent modifier have been investigated and aqueous standards were used for calibration. Pyrolysis and atomization temperatures were 600 °C and 1600 °C for the Pd-Mg modifier, and 500 °C and 1600 °C for Ir, respectively. The results obtained for Cd in the certified reference material NIST SRM 695 (Trace Elements in Multi-Nutrient Fertilizer) of 16.7 ± 1.3 μg g -1 and 16.4 ± 0.75 μg g -1 for the Pd-Mg and Ir modifier, respectively, were statistically not different from the certified value of 16.9 ± 0.2 μg g -1 on a 95% confidence level; however, the results obtained with the Ir modifier were significantly lower than those for the Pd-Mg modifier for most of the samples. The characteristic mass was 1.0 pg for the Pd-Mg modifier and 1.1 pg Cd for the Ir modifier, and the correlation coefficients (R 2) of the calibration were > 0.99. The instrumental limits of detection were 7.5 and 7.9 ng g -1, and the limits of quantification were 25 and 27 ng g -1 for Pd-Mg and Ir, respectively, based on a sample mass of 5 mg. The cadmium concentration in the investigated samples was between 0.07 and 5.5 μg g -1 Cd, and hence below the maximum value of 20 μg g -1 Cd permitted by Brazilian legislation.

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

    PubMed

    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

  20. Internal standardization in graphite furnace atomic absorption spectrometry: Comparative use of As and Ge to minimize matrix effects on Se determination in milk

    NASA Astrophysics Data System (ADS)

    Paiva de Oliveira, Adriana; Gomes Neto, José Anchieta; Nóbrega, Joaquim A.; Oliveira, Pedro Vitoriano

    2005-06-01

    Arsenic and germanium have been evaluated as internal standards to minimize matrix effects on the direct determination of selenium in milk by graphite furnace atomic absorption spectrometry (GFAAS) using tubes with integrated platform, pre-treated with W together with Pd as chemical modifier. The efficiency of As and Ge as internal standards for 25 μg L - 1 Se plus 500 μg L - 1 As or Ge in diluted (1 + 9 v/v) milk plus 1.0% (v/v) HNO 3 was evaluated by means of correlation graphs plotted from the normalized absorbance signals ( n = 20) of internal standard (axis y) versus analyte (axis x). The equations that describe the linear regression were: AAs = - 0.004 ± 0.019 + 1.02 ± 0.019 ASe ( r = 0.9967 ± 0.005); AGe = - 0.017 ± 0.015 + 1.01 ± 0.015 ASe ( r = 0.9978 ± 0.004). Samples and reference solutions were automatically spiked with 500 μg L - 1 Ge or As and 1.0% (v/v) HNO 3 by the autosampler. For 20 μL of aqueous standard solutions, analytical curves in the 5.00-40.0 μg L - 1 Se range were established using the ratio of Se absorbance to internal standard absorbance ( ASe / AIS) versus analyte concentration, and good linear correlations were obtained. The characteristic mass was 40 pg Se. Limits of detection were 0.55 and 0.40 μg L - 1 with As and Ge as the internal standard, respectively. Relative standard deviations (RSD) for a sample containing 25 μg L - 1 Se were 1.2% and 1.0% ( n = 12) using As and Ge, respectively. The RSD without internal standardization was about 6%. The accuracy of the proposed method was evaluated by an addition-recovery experiment and all recovered values were in the 99-105% range with IS and in the 70-80% range without IS. Using Ge as the internal standard, results of analysis of standard reference materials were in agreement with certified values at a 95% confidence level. The selenium concentration for 10 analyzed milk samples varied from 5.0 to 20 μg L - 1 .

  1. Activated electric arc furnace slag as an effective and reusable Fenton-like catalyst for the photodegradation of methylene blue and acid blue 29.

    PubMed

    Nasuha, N; Ismail, S; Hameed, B H

    2017-07-01

    In this work, an activated electric arc furnace slag (A-EAFS) was investigated as an effective Fenton catalyst for the photodegradation of methylene blue (MB) and acid blue 29 (AB29). Fourier transform infrared spectroscopy and UV-visible absorption analyses indicated that A-EAFS offers additional Fe3O4 because of the changes in the iron oxide phase and the favorable response to visible light. It has been found that the highest degradation efficiency can reach up to 94% for MB under optimal conditions of 1 g L(-1) of A-EAFS, 20 mM H2O2, and pH 3. The optimal conditions for AB29 were 0.1 g L(-1) A-EAFS, 4 mM H2O2, and pH 3 to reach 98% degradation efficiency. Visible light enhanced the degradation of both dyes. In addition, A-EAFS, could be easily separated magnetically, exhibited good chemical stability after seven successive photodegradation cycles. Copyright © 2017 Elsevier Ltd. All rights reserved.

  2. Synthesis of TiO2 visible light catalysts with controllable crystalline phase and morphology from Ti-bearing electric arc furnace molten slag.

    PubMed

    Li, Yang; Liu, Lulu; Guo, Min; Zhang, Mei

    2016-09-01

    TiO2 visible light catalysts with different crystalline phases and morphologies were synthesized from titanium-bearing electric arc furnace molten slag (Ti-bearing EAF slag) by using a simple acidolysis process. The effects of the pH of the HCl solution, liquid to solid ratio (RL/S, HCl solution to the residue ratio, mL/g) and acidolysis time on the micro-morphology and crystalline phase of as-prepared TiO2 photocatalysts were systematically investigated. The results indicated that with decreasing pH in the HCl solution and increasing RL/S, the crystalline phase and micro-morphology of the obtained TiO2 nanostructures tended to transform from anatase type TiO2 with spherical nanoparticle structures to rutile type TiO2 with needle-like nanorod structures. The acidolysis time had little influence on the crystalline phase but great impact on the size of the obtained TiO2. The growth mechanism of TiO2 from Ti-bearing EAF slag during the acidolysis process was also discussed. In addition, the influence of RL/S on the photocatalytic properties of the synthesized nanostructured TiO2 was studied. The results showed that the photodegradation efficiency for Rhodamine B solution could reach 91.00% in 120min when the RL/S was controlled at 50:1. Copyright © 2016. Published by Elsevier B.V.

  3. On the distribution and bonding environment of Zn and Fe in glasses containing electric arc furnace dust: a mu-XAFS and mu-XRF study.

    PubMed

    Pinakidou, F; Katsikini, M; Paloura, E C; Kavouras, P; Kehagias, Th; Komninou, Ph; Karakostas, Th; Erko, A

    2007-04-02

    We apply synchrotron radiation assisted X-ray fluorescence (SR-XRF), SR-XRF mapping as well as micro- and conventional X-ray absorption fine structure (mu-XAFS and XAFS) spectroscopies in order to study the bonding environment of Fe and Zn in vitrified samples that contain electric arc furnace dust from metal processing industries. The samples are studied in the as-cast state as well as after annealing at 900 degrees C. The SR-XRF results demonstrate that annealing does not induce any significant changes in the distribution of either Fe or Zn, in both the as-cast and annealed glasses. The mu-XAFS spectra recorded at the Fe-K and Zn-K edges reveal that the structural role of both Fe and Zn remains unaffected by the annealing procedure. More specifically, Fe forms both FeO(6) and FeO(4) polyhedra, i.e. acts as an intermediate oxide while Zn occupies tetrahedral sites.

  4. Chemical characterization of dust particles recovered from bag filters of electric arc furnaces for steelmaking: some factors influencing the formation of hexachlorobenzene.

    PubMed

    Tsubouchi, Naoto; Hashimoto, Hiroyuki; Ohtaka, Noriaki; Ohtsuka, Yasuo

    2010-11-15

    To make clear some factors controlling the formation of hexachlorobenzene (HCB) in the process of electric arc furnace (EAF) steelmaking, six dust samples recovered from different bag filters in commercial EAF steelmaking plants have been characterized with XRD, SEM-EPMA, XPS and temperature-programmed desorption (TPD) techniques. These dust samples contain 1.9-8.0 mass% of chlorine element, and the XPS and TPD measurements exhibit that the Cl is enriched at the dust surface and composed of the inorganic and organic functionalities, part of the Cl being evolved as HCl in the temperature region of flue gas treatment. All of the samples also include 2.1-6.4 mass% of carbon element, and some of the C can release CO(2) in the TPD up to 300°C to form active carbon sites. The number is related closely to HCB concentration of each dust. Further, it is suggested that the Zn present in the samples consists of ZnFe(2)O(4), ZnO and surface ZnCO(3), and the dust with a larger content of the ZnCO(3) has a higher concentration of HCB. It is possible that HCB formation occurs via gas-solid-solid interactions among gaseous Cl-containing compounds in flue gas, active carbon sites and surface Zn-species produced in exhaust ducts and bag filters.

  5. Freon (CHF3)-assisted atomization for the determination of titanium using ultrasonic slurry sampling-graphite furnace atomic absorption spectrometry (USS-GFAAS): a simple and advantageous method for solid samples.

    PubMed

    Asfaw, Alemayehu; Wibetoe, Grethe

    2004-06-01

    A simple and advantageous method for the determination of titanium using graphite furnace atomic absorption spectrometry with slurry sampling has been developed. Titanium is one of the refractory elements that form thermally stable carbides in the graphite tube, which leads to severe memory effects. Trifluoromethane (Freon-23) was applied in the purge gas during the atomization step or alternatively just prior to the atomization to successfully eliminate the problems of carbide formation and increase the lifetime of the furnace tube which could be used for more than 600 heating cycles. A flow rate of 40 mL min(-1) (5% of Freon in argon) was used to obtain symmetrical peaks with no tailing. However, when the gas flow rate was too high (250 mL min(-1)) the peak-tailing and memory effects reappeared. Ti was determined in various materials covering a wide range of concentrations, from 2.8 microg g(-1) to 12% (m/m) Ti. The accuracy of the method was confirmed by analyzing certified reference materials (CRMs) or by comparing the results with those obtained using inductively coupled plasma-atomic emission spectrometry (ICP-AES) after decomposition of the samples. The materials analyzed were soil, plant, human hair, coal, urban particulate matters, toothpaste, and powdered paint.

  6. Highly sensitive determination of cadmium and lead in leached solutions from ceramic ware by graphite furnace atomic absorption spectrometry coupled with sequential injection-based solid phase extraction method.

    PubMed

    Ueda, Minoru; Teshima, Norio; Sakai, Tadao; Joichi, Yasutaka; Motomizu, Shoji

    2010-01-01

    A fully automated pretreatment system based on sequential injection solid-phase extraction (SPE) coupled to a graphite furnace atomic absorption spectrometer (Auto-Pret-GFAAS system) was developed to determine trace amounts of cadmium and lead. A handmade minicolumn packed with a chelating resin was used for the preconcentration of both metals. All protocol for the on-line SPE method was controlled by home-made software. A trigger switch that was placed next to the graphite furnace was used to synchronize the home-made software with built-in software in the GFAAS. One milliliter of sample solution was flowed through into the minicolumn, the analytes were collected and concentrated on the solid phase, and the analytes were eluted with nitric acid (3 M), and detected by GFAAS. The limits of detection (3sigma) for cadmium and lead were 0.20 and 2.6 ng L(-1), respectively. The sample throughput was 47 h(-1) for 1 mL sample loading. The proposed sensitive method with the original Auto-Pret-GFAAS system was applied to the determination of cadmium and lead in tap water and in leached solutions from ceramic ware using 4% acetic acid.

  7. Characterisation of the sintering behaviour of Waelz slag from electric arc furnace (EAF) dust recycling for use in the clay ceramics industry.

    PubMed

    Quijorna, N; de Pedro, M; Romero, M; Andrés, A

    2014-01-01

    Waelz slag is an industrial by-product from the recovery of electric arc furnace (EAF) dust which is mainly sent to landfills. Despite the different chemical and mineralogical compositions of Waelz slag compared to traditional clays, previous experiments have demonstrated its potential use as a clay substitute in ceramic processes. Indeed, clayey products containing Waelz slag could improve mechanical and environmental performance, fixing most of the metallic species and moreover decreasing the release of some potential pollutants during firing. However, a deeper understanding of the complex phase transformations during its thermal treatment and the connection of this behaviour with the end properties is desirable in order to explain the role that is played by the Waelz slag and its potential contribution to the ceramic process. For this purpose, in the present study, the chemical, mineralogical, thermal and environmental behaviour of both (i) unfired powdered samples, and (ii) pressed specimen of Waelz slag fired up to different temperatures within the typical range of clay based ceramic production, has been studied. The effect of the heating temperature on the end properties of the fired samples has been assessed. In general, an increase of the firing temperature promotes sintering and densification of the products and decreases the open porosity and water absorption which also contributes to the fixation of heavy metals. On the contrary, an increase in the leaching of Pb, Cr and Mo from the fired specimens is observed. This can be attributed to the creation of Fe and Ca molybdates and chromates that are weakly retained in the alkali matrix. On the other side, at temperature above 950 °C a weight gain related to the emission of evolved gases is observed. In conclusion, the firing temperature of the ceramic process is a key parameter that affects not only the technical properties but also strongly affects the leaching behaviour and the process emissions.

  8. Vacuum Melting of Refractory Metals and Alloys in Lining Furnaces (Chapter VI),

    DTIC Science & Technology

    Melting, *Refractory metals, *Refractory metal alloys, Vacuum furnaces, Linings, Electric arcs, Crucibles, Titanium alloys, Safety, Arc melting, Electron beam melting , Plasmas(Physics), Heating, Translations, USSR

  9. Characterization and comparison of vanadyl and nickel compounds in heavy crude petroleums and asphaltenes by reverse-phase and size-exclusion liquid chromatography/graphite furnace atomic absorption spectrometry

    SciTech Connect

    Fish, R.H.; Komlenic, J.J.; Wines, B.K.

    1984-11-01

    Vanadyl and nickel non-porphyrin rich fractions have been characterized in pyridine/water extracts of four heavy crude petroleums using reverse-phase high-performance liquid chromatography in combination with element-selective graphite furnace atomic absorption detection (RP-HPLC/GFAA). On the basis of rapid-scan UV-vis data indicating a lack of Soret absorbance associated with separated vanadyl and nickel containing fractions, we have categorized highly polar nickel compounds as non-porphyrin in Boscan, Cerro Negro, Wilmington, and Prudhoe Bay heavy crude petroleums. The presence of lower polarity vanadyl non-porphyrin compounds, occurring primarily in Wilmington and Prudhoe Bay petroleum, has also been confirmed. The vanadium histogrammic profiles, obtained using reverse-phase and size-exclusion HPLC/GFAA analysis for compounds extracted from the n-pentane (40:1) precipitated asphaltenes, were similar when compared to the pyridine/water extracts from the heavy crude petroleums.

  10. 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.

    PubMed

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

    2009-02-15

    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 1.0molL(-1) HNO(3) was used as eluent. The metal ions in 300mL solution can be concentrated to 1.0mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0g 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 1.4ngL(-1) for Cr(III), 1.0ngL(-1) for Ni(II), 0.85ngL(-1) for Ag(I), 1.2ngL(-1) for Co(II), 1.0ngL(-1) for Cu(II), 1.2ngL(-1) for Cd(II) and 1.3ngL(-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).

  11. Exposure assessment of workers to airborne PCDD/Fs, PCBs and PAHs at an electric arc furnace steelmaking plant in the UK.

    PubMed

    Aries, Eric; Anderson, David R; Fisher, Raymond

    2008-06-01

    Occupational exposure studies were undertaken at a UK electric arc furnace (EAF) steelmaking plant to investigate the exposure of workers via inhalation to dioxins, polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs) including benzo[a]pyrene (B[a]P). Surveys were undertaken in areas including the melting shop, the casting department and a furnace control cabin. The highest concentrations of dioxins and PCBs were found inside the melting shop nearby EAFs, whereas dioxin and PCB concentrations in the casting department and inside the control cabin were significantly lower. Risk characterization was carried out by comparing the daily intake of dioxins and PCBs through inhalation with the recommended tolerable daily intake (TDI). Health risk assessments were also carried out by combining exposure data with inhalation cancer potency factors to quantify the cancer risk. For the most exposed category of workers (melting shop workers), the estimated daily intake via inhalation was 0.35 pg WHO-TEQ kg(-1) body weight (bw) in the worst case scenario. Considering that the average UK adult exposure to dioxins from the diet is 1.8 pg WHO-TEQ kg(-1) bw day(-1), the results indicated that the estimated daily intake of dioxins via inhalation at the EAF would not result in the recommended range of the TDI (1-4 pg WHO-TEQ kg(-1) bw day(-1)) being exceeded. Cancer risks for a 40-year occupational exposure period were determined by multiplying the inhalation dose by the inhalation cancer potency factor for 2,3,7,8-tetrachlorodibenzo-p-dioxin. For melting shop workers, cancer risks from exposure to dioxins and PCBs ranged from 2.05 x 10(-5) to 7.54 x 10(-5). Under most regulatory programmes, excess cancer risks between 1.0 x 10(-4) and 1.0 x 10(-6) indicate an acceptable range of excess cancer risk, suggesting a limited risk from dioxin exposure for workers in the EAF plant. For the calculation of excess cancer risks, no account has been taken of the protection

  12. Metals purification by improved vacuum arc remelting

    DOEpatents

    Zanner, Frank J.; Williamson, Rodney L.; Smith, Mark F.

    1994-12-13

    The invention relates to improved apparatuses and methods for remelting metal alloys in furnaces, particularly consumable electrode vacuum arc furnaces. Excited reactive gas is injected into a stationary furnace arc zone, thus accelerating the reduction reactions which purify the metal being melted. Additionally, a cooled condensation surface is disposed within the furnace to reduce the partial pressure of water in the furnace, which also fosters the reduction reactions which result in a purer produced ingot. Methods and means are provided for maintaining the stationary arc zone, thereby reducing the opportunity for contaminants evaporated from the arc zone to be reintroduced into the produced ingot.

  13. Brazing graphite to graphite

    DOEpatents

    Peterson, George R.

    1976-01-01

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

  14. Calculation of net emission coefficient of electrical discharge machining arc plasmas in mixtures of nitrogen with graphite, copper and tungsten

    NASA Astrophysics Data System (ADS)

    Adineh, V. R.; Coufal, O.; Bartlova, M.

    2015-10-01

    This work reports theoretical calculations of electrical discharge machining (EDM) radiative properties for mixture systems of N2-C, N2-Cu and N2-W arc plasmas, in the temperature range of 3000-10 000 K, and at 1 and 10 bar pressures. Radiative properties are computed for various plasma sizes as well as vapour proportions. Calculations consider line overlapping with spectrum coverage from 30 to 10 000 nm. Doppler, Natural, Van-der-Waals, Resonance and Stark broadening are taken into account as the line broadening mechanisms. Besides, continuum calculations consider bound-free and free-free emissions along with molecular bands radiation for selected molecular systems. Results show that contamination vapours of EDM electrode have strong influence on the amount of EDM plasma radiation to the surrounding environment. However, comparison of impurities from workpiece with electrode one indicates that Fe vapour has stronger impact on modifying the EDM arc plasma radiative properties, compared to the C, Cu and W species studied in this research.

  15. High temperature furnace modeling and performance verifications

    NASA Technical Reports Server (NTRS)

    Smith, James E., Jr.

    1992-01-01

    Analytical, numerical, and experimental studies were performed on two classes of high temperature materials processing sources for their potential use as directional solidification furnaces. The research concentrated on a commercially available high temperature furnace using a zirconia ceramic tube as the heating element and an Arc Furnace based on a tube welder. The first objective was to assemble the zirconia furnace and construct parts needed to successfully perform experiments. The 2nd objective was to evaluate the zirconia furnace performance as a directional solidification furnace element. The 3rd objective was to establish a data base on materials used in the furnace construction, with particular emphasis on emissivities, transmissivities, and absorptivities as functions of wavelength and temperature. A 1-D and 2-D spectral radiation heat transfer model was developed for comparison with standard modeling techniques, and were used to predict wall and crucible temperatures. The 4th objective addressed the development of a SINDA model for the Arc Furnace and was used to design sample holders and to estimate cooling media temperatures for the steady state operation of the furnace. And, the 5th objective addressed the initial performance evaluation of the Arc Furnace and associated equipment for directional solidification. Results of these objectives are presented.

  16. High temperature furnace modeling and performance verifications

    NASA Technical Reports Server (NTRS)

    Smith, James E., Jr.

    1988-01-01

    Analytical, numerical and experimental studies were performed on two classes of high temperature materials processing furnaces. The research concentrates on a commercially available high temperature furnace using zirconia as the heating element and an arc furnace based on a ST International tube welder. The zirconia furnace was delivered and work is progressing on schedule. The work on the arc furnace was initially stalled due to the unavailability of the NASA prototype, which is actively being tested aboard the KC-135 experimental aircraft. A proposal was written and funded to purchase an additional arc welder to alleviate this problem. The ST International weld head and power supply were received and testing will begin in early November. The first 6 months of the grant are covered.

  17. Ferrosilicon smelting in a direct current furnace

    DOEpatents

    Dosaj, Vishu D.; May, James B.

    1992-12-29

    The present invention is a process for smelting ferrosilicon alloy. The process comprises adding a carbon source and tailings comprising oxides of silicon and iron to a substantially closed furnace. Heat is supplied to the furnace by striking a direct current arc between a cathode electrode and an anode functional hearth. In a preferred embodiment of the present invention, the cathode electrode is hollow and feed to the substantially closed furnace is through the hollow electrode.

  18. Ferrosilicon smelting in a direct current furnace

    DOEpatents

    Dosaj, V.D.; May, J.B.

    1992-12-29

    The present invention is a process for smelting ferrosilicon alloy. The process comprises adding a carbon source and tailings comprising oxides of silicon and iron to a substantially closed furnace. Heat is supplied to the furnace by striking a direct current arc between a cathode electrode and an anode functional hearth. In a preferred embodiment of the present invention, the cathode electrode is hollow and feed to the substantially closed furnace is through the hollow electrode. 1 figure.

  19. Volt-ampere characteristics of a nitrogen DC plasma arc with anode melting

    NASA Astrophysics Data System (ADS)

    Zhao, Peng; Ni, Guo-Hua; Meng, Yue-Dong; Nagatsu, Masaaki

    2013-06-01

    The characteristics of a nitrogen arc using a graphite cathode and a melting anode in a pilot-scale plasma furnace are investigated. The voltage is examined as a function of current and apparent plasma length. The voltage increases non-linearly with the increase of apparent plasma length, with the current fixed. The experimental data so obtained are compared with the predictions of the Bowman model for the electric arc, and with numerical simulations as well. The level of agreement between the experimental data at the melting anode and the numerical predictions confirms the suitability of the proposed the Bowman model. These characteristics are relevant to the engineering design and evaluation of a DC plasma furnace and reactor for the treatment of hazardous fly ash waste.

  20. Preparation and characterization of magnetic nanoparticles for the on-line determination of gold, palladium, and platinum in mine samples based on flow injection micro-column preconcentration coupled with graphite furnace atomic absorption spectrometry.

    PubMed

    Ye, Juanjuan; Liu, Shuxia; Tian, Miaomiao; Li, Wanjun; Hu, Bin; Zhou, Weihong; Jia, Qiong

    2014-01-01

    A simple and highly selective procedure for on-line determination of trace levels of Au, Pd, and Pt in mine samples has been developed using flow injection-column adsorption preconcentration coupled with graphite furnace atomic absorption spectrophotometry (FI-column-GFAAS). The precious metals were adsorbed on the as-synthesized magnetic nanoparticles functionalized with 4'-aminobenzo-15-crown-5-ether packed into a micro-column and then eluted with 2% thiourea + 0.1 mol L(-1) HCl solution prior to the determination by GFAAS. The properties of the magnetic adsorbents were investigated by scanning electron microscope (SEM), X-ray diffraction (XRD), and vibrating sample magnetometer (VSM). Various experimental parameters affecting the preconcentration of Au, Pd, and Pt were investigated and optimized. Under the optimal experimental conditions, the detection limits of the developed technique were 0.16 ng mL(-1) for Au, 0.28 ng mL(-1) for Pd, and 1.01 ng mL(-1) for Pt, with enrichment factors of 24.3, 13.9, and 17.8, respectively. Precisions, evaluated as repeatability of results, were 1.1%, 3.9%, and 4.4% respectively for Au, Pd, and Pt. The developed method was validated by the analysis of Au, Pd, and Pt in certified reference materials and mine samples with satisfactory results.

  1. 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.

    PubMed

    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.

  2. 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.

    PubMed

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

    2014-02-17

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

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

    NASA Astrophysics Data System (ADS)

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

    2017-06-01

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

  4. Displacement-dispersive liquid-liquid microextraction based on solidification of floating organic drop of trace amounts of palladium in water and road dust samples prior to graphite furnace atomic absorption spectrometry determination.

    PubMed

    Ghanbarian, Maryam; Afzali, Daryoush; Mostafavi, Ali; Fathirad, Fariba

    2013-01-01

    A new displacement-dispersive liquid-liquid microextraction method based on the solidification of floating organic drop was developed for separation and preconcentration of Pd(ll) in road dust and aqueous samples. This method involves two steps of dispersive liquid-liquid microextraction based on solidification. In Step 1, Cu ions react with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which is extracted by dispersive liquid-liquid microextraction based on a solidification procedure using 1-undecanol (extraction solvent) and ethanol (dispersive solvent). In Step 2, the extracted complex is first dispersed using ethanol in a sample solution containing Pd ions, then a dispersive liquid-liquid microextraction based on a solidification procedure is performed creating an organic drop. In this step, Pd(ll) replaces Cu(ll) from the pre-extracted Cu-DDTC complex and goes into the extraction solvent phase. Finally, the Pd(ll)-containing drop is introduced into a graphite furnace using a microsyringe, and Pd(ll) is determined using atomic absorption spectrometry. Several factors that influence the extraction efficiency of Pd and its subsequent determination, such as extraction and dispersive solvent type and volume, pH of sample solution, centrifugation time, and concentration of DDTC, are optimized.

  5. Zincon-immobilized silica-coated magnetic Fe3O4 nanoparticles for solid-phase extraction and determination of trace lead in natural and drinking waters by graphite furnace atomic absorption spectrometry.

    PubMed

    Jiang, Hong-mei; Yan, Zhong-peng; Zhao, Yue; Hu, Xin; Lian, Hong-zhen

    2012-05-30

    A new protocol using zincon-immobilized silica-coated magnetic Fe(3)O(4) nanoparticles (Zincon-Si-MNPs) as solid-phase extraction (SPE) medium has been developed for the separation and preconcentration of trace lead in water. Various parameters such as pH, extraction time, concentration and volume of eluent, sample volume, and influence of co-existing ions have been investigated in order to establish the optimum conditions for the determination of lead in combination with graphite furnace atomic absorption spectrometry (GFAAS). The detection limit (LOD) of the proposed method for lead based on an enrichment factor of 200 was 10 ng L(-1). The relative standard deviations (RSDs, n=5) were 8.3%, 7.8% and 9.2%, respectively, at 5, 0.5 and 0.05 ng mL(-1) levels. This method has been successfully applied to the analysis of trace lead in natural and drinking water samples and the recoveries for the spiked samples were in the range of 84-104%.

  6. 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.

    PubMed

    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.

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

    PubMed

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

    2016-04-01

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

  8. Comparison of closed-vessel and focused open-vessel microwave dissolution for determination of cadmium, copper, lead, and selenium in wheat, wheat products, corn bran, and rice flour by transverse-heated graphite furnace atomic absorption spectrometry.

    PubMed

    Gawalko, E J; Nowicki, T W; Babb, J; Tkachuk, R; Wu, S

    1997-01-01

    A method is described for the determination of Pb, Cd, Cu, and Se in cereal samples. An atomic absorption spectrometer equipped with a transverse-heated graphite furnace with Zeeman background correction was used for all determinations. Sample preparation was performed by closed-vessel microwave digestion using nitric acid and focused openvessel microwave digestion using nitric acid-hydrogen peroxide. Both techniques were evaluated by using 15 cereal reference materials and comparing results with certified or reference values for each element. Cereal reference standards obtained from the Community Bureau of Reference (Europe), the National Institute of Standards and Technology (USA), the National Institute for Environmental Studies (Japan), the National Research Centre for Certified Reference Materials (People's Republic of China), and the Canadian Grain Commission were used. Application of a series of t-tests, conducted according to Sidak's modified Bonerroni t-procedure, showed that both techniques yielded accurate results for cereal reference materials. Some differences from certified and reference values, however, were found for each element.

  9. Use of a novel medium, the ionic liquid 1-butyl-3-trimethylsilylimidazolium hexafluorophosphate, for liquid-liquid extraction of lead in water and its determination by graphite furnace atomic absorption spectrometry.

    PubMed

    Zaijun, Li; Qiping, Peng; Haixia, Shan

    2007-01-01

    The ionic liquid 1-butyl-3-trimethylsilylimidazolium hexafluorophosphate, abbreviated as [C4tmsim][PF6], was developed as a novel medium for liquid-liquid extraction of lead(II) in water, in which dithizone was used as a metal chelator to form a neutral lead-dithizone complex. Under optimal conditions, the complex was extracted into the [C4tmsim][PF6] phase from aqueous solution and back-extracted with nitric acid solution into the aqueous phase that was used directly for the subsequent determination of Pb. The system using the ionic liquid demonstrated good extraction performance; the extraction and back-extraction efficiencies were 99.8 and 99.7%, respectively, for Pb(II) at 20 microg/L. The above procedure, including the extraction and back-extraction, was used to enrich trace levels of Pb(ll) in a relatively large volume of water samples (1000 mL water), and an enrichment factor of 400 was obtained. The enrichment coupled with graphite furnace atomic absorption spectrometry was successfully applied to the determination of Pb in water. The calibration graph was linear at levels near the detection limits up to > or = 100 ng/L Pb(II). The limits of quantitation and detection for lead in real water samples were 2.5 and 1.0 ng/L, respectively. Lead recoveries of 96.2-103.8% from spiked samples demonstrate the accuracy of the proposed method.

  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

    NASA Astrophysics Data System (ADS)

    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. Determination of total selenium content in sediments and natural water by graphite furnace-atomic absorption spectroscopy after collection as a selenium(IV) complex on activated carbon.

    PubMed

    Kubota, T; Suzuki, K; Okutani, T

    1995-07-01

    A trace level of Se was collected on activated carbon (AC) as the Se(IV)-3-phenyl-5-mercapto-1,3,4-thiadiazole-2(3H)-thione (Bismuthiol II) complex. The AC was directly introduced as an AC-suspension into the graphite tube atomizer and the Se concentration was determined by atomic absorption spectroscopy (T. Okutani, T. Kubota, N. Sugiyama and Y. Turuta, Nippon Kagaku Kaishi, (1991) 375). The amount of Se in heavily contaminated samples including sediment, lake water and seawater was determined using this method. The sediments were digested with HNO(3)HClO(4)HF and the interference from AlF(3) was removed using H(3)BO(3)HClO(4). Lake water and seawater were acidified with H(2)SO(4) and digested with KMnO(4). The Se concentrations of these samples were determined by this method with satisfactory results. The above method is simple, rapid and applicable to heavily contaminated samples.

  12. Fast emulsion-based method for simultaneous determination of Co, Cu, Pb and Se in crude oil, gasoline and diesel by graphite furnace atomic absorption spectrometry.

    PubMed

    Luz, Maciel S; Nascimento, Angerson N; Oliveira, Pedro V

    2013-10-15

    A method for the simultaneous determination of Co, Cu, Pb and Se in crude oil, gasoline and diesel samples using emulsion-based sampling and GF AAS is proposed. 400mg of sample was weighted in volumetric flask following the sequential addition of 125 µL of hexane and 7.5 mL of Triton X-100(®) (20% mv(-1)). Subsequently, the mixture was stirred in ultrasonic bath, during 30 min, before dilution to 25 mL with deionized water. Aliquots of 20 μL of reference solution or sample emulsion were co-injected into the graphite tube with 10 μL of 2 g L(-1) Pd(NO3)2. The pyrolysis and atomization temperatures were 1300°C and 2250°C, respectively. The limits of detection (n=10, 3σ) and characteristic masses were 0.02 μg g(-1) (0.32 μg L(-1)) and 18 pg for Co, 0.03 μg g(-1) (0.48 μg L(-1)) and 15 pg for Cu, 0.04 μg g(-1) (0.64 μg L(-1)) and 48 pg for Pb, and 0.11 μg g(-1) (1.76 μg L(-1)) and 47 pg for Se. The reliabilities of the proposed method for Co and Se were checked by SRM(®) 1634c Residual Oil analysis. The found values are in accordance to the SRM at 95% confidence level (Student's t-test). Each sample was spiked with 0.18 μg g(-1) of Co, Cu, Pb and Se and the recoveries varied from 92% to 116% for Co, 83% to 117% for Cu, 72% to 117% for Pb, and 82% to 122% for Se.

  13. Study on the effects of nitrilotriproprionic acid and 4,5-dihydroxy-1,3-benzene disulphonate on the fractionation of beryllium in human serum using graphite furnace atomic absorption spectrometry

    PubMed Central

    Stephan, Chadi H; Fournier, Michel; Brousseau, Pauline; Sauvé, Sébastien

    2008-01-01

    Background Occupational exposure to beryllium may cause Chronic Beryllium Disease (CBD), a lung disorder initiated by an electrostatic interaction with the MHC class II human leukocyte antigen (HLA). Molecular studies have found a significant correlation between the electrostatic potential at the HLA-DP surface and disease susceptibility. CBD can therefore be treated by chelation therapy. In this work, we studied the effect of two complexing agents, nitrilotriproprionic acid (NTP) and 4,5-dihydroxy-1,3-benzene disulphonate (Tiron), on the fractionation of beryllium in human serum analysed by graphite furnace atomic absorption spectrometry (GFAAS). Results We found the average serum beryllium concentration of fourteen non-exposed individuals to be 0.53 (± 0.14) μg l-1, with 21 (± 3)% of the beryllium mass bound to the low molecular weight fraction (LMW), and 79 (± 3)% bound to the high molecular weight fraction (HMW). The addition of Tiron increased the beryllium mass in the HMW fraction, while NTP was not seen to have any influence on the fractionation of beryllium between the two fractions. NTP was, however, shown to complex 94.5% of the Be mass in the LMW fraction. The beryllium GFAAS detection limit, calculated as three times the standard deviation of 10 replicates of the lowest standard (0.05 μg L-1), was 6.0 (± 0.2) ng L-1. Conclusion The concentration of beryllium or its fractionation in human serum was not affected by sex or smoking habit. On average, three quarters of the beryllium in serum were found in the HMW fraction. Of the two ligands tested, only Tiron was effective in mobilising beryllium under physiological conditions, thus increasing the Be content in the HMW fraction. PMID:18479524

  14. 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.

    PubMed

    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).

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

    PubMed

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

    2016-12-01

    Different precursors were evaluated for the generation of reference spectra and correction of the background caused by SiO molecules in the determination of Sb in facial cosmetics by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis. Zeolite and mica were the most effective precursors for background correction during Sb determination using the 217.581nm and 231.147nm lines. Full 2(3) factorial design and central composite design were used to optimize the atomizer temperature program. The optimum pyrolysis and atomization temperatures were 1500 and 2100°C, respectively. A Pd(NO3)2/Mg(NO3)2 mixture was employed as the chemical modifier, and calibration was performed at 217.581nm with aqueous standards containing Sb in the range 0.5-2.25ng, resulting in a correlation coefficient of 0.9995 and a slope of 0.1548s ng(-1). The sample mass was in the range 0.15-0.25mg. The accuracy of the method was determined by analysis of Montana Soil (II) certified reference material, together with addition/recovery tests. The Sb concentration found was in agreement with the certified value, at a 95% confidence level (paired t-test). Recoveries of Sb added to the samples were in the range 82-108%. The limit of quantification was 0.9mgkg(-1) and the relative standard deviation (n=3) ranged from 0.5% to 7.1%. From thirteen analyzed samples, Sb was not detected in ten samples (blush, eye shadow and compact powder); three samples (two blush and one eye shadow) presented Sb concentration in the 9.1-14.5mgkg(-1) range.

  16. Determination of calcium by inductively coupled plasma-atomic emission spectrometry, and lead by graphite furnace atomic absorption spectrometry, in calcium supplements after microwave dissolution or dry-ash digestion: method trial.

    PubMed

    Siitonen, P H; Thompson, H C

    1998-01-01

    A 3-laboratory method trial was conducted to evaluate 2 sample digestion procedures and instrumental determination parameters for analysis of calcium and lead in Ca supplements. Calcium supplements were treated by dry-ash digestion or microwave dissolution prior to spectrometric analysis. In each case, Pb was determined by graphite furnace atomic absorption spectrometry and Ca by inductively coupled plasma-atomic emission spectrometry. Blind duplicates of 6 Ca supplement samples were analyzed after each sample treatment procedure. Matrix pairs contained dissimilar Pb levels to cover the analyte range encountered during method development. Calcium content of the Ca supplement samples also reflected the range seen during method development. Stock solutions of Ca and Pb were supplied to collaborators for preparation of quantitation standards to remove a variable external to the method. National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1486, bone meal, was included to assess method accuracy and recovery at NIST certificate Ca and Pb levels for this material (26.58 +/- 0.24% Ca and 1.335 +/- 0.014 micrograms Pb/g). Analyses of the NIST SRM yielded 25.9 +/- 1.1 and 27.2 +/- 2.3% Ca and 1.53 +/- 0.19 and 1.26 +/- 0.19 micrograms Pb/g for dry-ash and microwave procedures, respectively. Statistical analyses of data indicated acceptable repeatability and reproducibility for determination of Pb and Ca in various Ca supplements. With either sample preparation technique, the method is appropriate for determining Pb or Ca in Ca supplements.

  17. Evaluation of Bi as internal standard to minimize matrix effects on the direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry using Ru permanent modifier with co-injection of Pd/Mg(NO 3) 2

    NASA Astrophysics Data System (ADS)

    de Oliveira, Silvana Ruella; Neto, José Anchieta Gomes

    2007-09-01

    Bismuth was evaluated as an internal standard for the direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry using Ru as a permanent modifier with co-injection of Pd/Mg(NO 3) 2. The correlation coefficient of the graph plotted from the normalized absorbance signals of Bi versus Pb was r = 0.989. Matrix effects were evaluated by analyzing the slope ratios between the analytical curve obtained from reference solutions prepared in 0.2% (v/v) HNO 3 and analytical curves obtained from Pb additions in red and white wine vinegar samples. The calculated ratios were around 1.04 and 1.02 for analytical curves established applying an internal standard and 1.3 and 1.5 for analytical curves without. Analytical curves in the 2.5-15 μg L - 1 Pb concentration interval were established using the ratio Pb absorbance to Bi absorbance versus analyte concentration, and typical linear correlations of r = 0.999 were obtained. The proposed method was applied for direct determination of Pb in 18 commercial vinegar samples and the Pb concentration varied from 2.6 to 31 μg L - 1 . Results were in agreement at a 95% confidence level (paired t-test) with those obtained for digested samples. Recoveries of Pb added to vinegars varied from 96 to 108% with and from 72 to 86% without an internal standard. Two water standard reference materials diluted in vinegar sample were also analyzed and results were in agreement with certified values at a 95% confidence level. The characteristic mass was 40 pg Pb and the useful lifetime of the tube was around 1600 firings. The limit of detection was 0.3 μg L - 1 and the relative standard deviation was ≤ 3.8% and ≤ 8.3% ( n = 12) for a sample containing 10 μg L - 1 Pb with and without internal standard, respectively.

  18. A novel approach in dispersive liquid-liquid microextraction based on the use of an auxiliary solvent for adjustment of density UV-VIS spectrophotometric and graphite furnace atomic absorption spectrometric determination of gold based on ion pair formation.

    PubMed

    Kocúrová, Lívia; Balogh, Ioseph S; Skrlíková, Jana; Posta, József; Andruch, Vasil

    2010-10-15

    This paper presents a novel approach to dispersive liquid-liquid microextraction (DLLME), based on the use of an auxiliary solvent for the adjustment of density. The procedure utilises a solvent system consisting of a dispersive solvent, an extraction solvent and an auxiliary solvent, which allows for the use of solvents having a density lower than that of water as an extraction solvent while preserving simple phase separation by centrifugation. The suggested approach could be an alternative to procedures described in the literature in recent months and which have been devoted to solving the same problem. The efficiency of the suggested approach is demonstrated through the determination of gold based on the formation of the ion pair [Au(CN)(2)](-) anion with Astra Phloxine (R) reagent and its extraction using the DLLME procedure with subsequent UV-VIS spectrophotometric and graphite furnace atomic absorption spectrometric detection. The optimum conditions were found to be: pH 3; 0.8 mmol L(-1) K(4)[Fe(CN)(6)]; 0.12 mmol L(-1) R; dispersive solvent, methanol; extraction solvent, toluene; auxiliary solvent, tetrachloromethane. The calibration plots were linear in the ranges 0.39-4.7 mg L(-1) and 0.5-39.4 μg L(-1) for UV-VIS and GFAAS detection, respectively; thus enables the application of the developed method in two ranges differing from one from another by three orders of magnitude. The presented approach can be applied to the development of DLLME procedures for the determination of other compounds extractable by organic solvents with a density lower than that of water. Copyright © 2010 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

    NASA Astrophysics Data System (ADS)

    Resano, Martín; Flórez, María del Rosario; Queralt, Ignasi; Marguí, Eva

    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 (NH4F·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- 1 (Pd), 8.3 μg g- 1 (Pt) and 9.3 μg g- 1 (Rh) for catalysts, which decreased to 0.08 μg g- 1 (Pd), 0.15 μg g- 1 (Pt) and 0.10 μg g- 1 (Rh) for pharmaceuticals.

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

    PubMed

    Amiri, Mojtaba; Amini, Ramin

    2012-08-01

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

  1. Speciation of nickel in airborne particulate matter by means of sequential extraction in a micro flow system and determination by graphite furnace atomic absorption spectrometry and inductively coupled plasma mass spectrometry.

    PubMed

    Fuichtjohann, L; Jakubowski, N; Gladtke, D; Klocko, D; Broekaert, J A

    2001-12-01

    A four-stage sequential extraction procedure for the speciation of nickel has been applied to ambient aerosol samples. The determination of the soluble, sulfidic, metallic and oxidic Ni fractions in particulate matter was carried out by graphite furnace (electrothermal) atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). An EDTA solution, a mixture of diammonium citrate and hydrogen peroxide, and a KCuCl3 solution were used as leaching agents for the determination of the soluble, sulfidic and metallic species, respectively, and nitric acid was used for the determination of oxidic compounds after microwave digestion of particulate matter sampled on filters. A new micro scale filter holder placed in a closed flow injection analysis (FIA) system for use in nickel speciation by means of sequential extraction, and the results of the optimisation of the extraction conditions are described. The temperature program for ETAAS was optimised for all extraction solutions with the aid of temperature curves. Pyrolysis temperatures of 900. 600 and 1,000 degrees C were found to be optimum for EDTA, hydrogen peroxide plus ammonium citrate and KCuCl3-containing solutions, respectively. Airborne dust was sampled on lilters at two locations near to a metallurgical plant in Dortmund, Germany. Concentrations in the low ng m(-3) range down to the detections limits (0.1-0.3 ng m(-3)) and various nickel species were found to be present in the collected dust. The mean fractions of total nickel (sampling period of one month) were found to contain 36+20% of soluble, 6 +/- 4% of sulfidic, 11 +/- 15% of metallic and 48 +/- 18% of oxidic nickel.

  2. 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.

    PubMed

    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%).

  3. Tube furnace

    DOEpatents

    Foster, Kenneth G.; Frohwein, Eugene J.; Taylor, Robert W.; Bowen, David W.

    1991-01-01

    A vermiculite insulated tube furnace is heated by a helically-wound resistance wire positioned within a helical groove on the surface of a ceramic cylinder, that in turn is surroundingly disposed about a doubly slotted stainless steel cylindrical liner. For uniform heating, the pitch of the helix is of shorter length over the two end portions of the ceramic cylinder. The furnace is of large volume, provides uniform temperature, offers an extremely precise programmed heating capability, features very rapid cool-down, and has a modest electrical power requirement.

  4. Tube furnace

    SciTech Connect

    Foster, K.G.; Frohwein, E.J.; Taylor, R.W.; Bowen, D.W.

    1990-12-31

    A vermiculite insulated tube furnace is heated by a helically-wound resistance wire positioned within a helical groove on the surface of a ceramic cylinder, that in turn is surroundingly disposed about a doubly slotted stainless steel cylindrical liner. For uniform heating, the pitch of the helix is of shorter length over the two end portions of the ceramic cylinder. The furnace is of large volume, provides uniform temperature, offers an extremely precise programmed heating capability, features very rapid cool-down, and has a modest electrical power requirement.

  5. Tube furnace

    SciTech Connect

    Foster, K.G.; Frohwein, E.J.; Taylor, R.W.; Bowen, D.W.

    1990-01-01

    A vermiculite insulated tube furnace is heated by a helically-wound resistance wire positioned within a helical groove on the surface of a ceramic cylinder, that in turn is surroundingly disposed about a doubly slotted stainless steel cylindrical liner. For uniform heating, the pitch of the helix is of shorter length over the two end portions of the ceramic cylinder. The furnace is of large volume, provides uniform temperature, offers an extremely precise programmed heating capability, features very rapid cool-down, and has a modest electrical power requirement.

  6. Graphite millimeter-wave waveguide and mirror for high temperature environments

    SciTech Connect

    Woskov, P.P.; Titus, C.H.

    1995-12-01

    A graphite helix corrugated waveguide with a miter mirror has been fabricated and used for 135 GHz pyrometer measurements on a high temperature plasma arc furnace. The guide has an internal diameter of 3.81 cm, a length of 123 cm, and a corrugation of 32 grooves/inch. One end of the guide was sealed with a Teflon window having moth eye surfaces to reduce reflections.The room temperature insertion loss of this guide assembly for HE{sub 11} mode propagation and launch was measured to be 0.5 {+-} 0.1 dB. It was used successfully in a high temperature environment where the miter mirror end reached incandescent temperatures in access of 1,200 C. High temperature graphite surface corrosion typically increased the insertion loss to 1.2 {+-} 0.2 dB but did not significantly affect the beam divergence.

  7. Furnace assembly

    DOEpatents

    Panayotou, Nicholas F.; Green, Donald R.; Price, Larry S.

    1985-01-01

    A method of and apparatus for heating test specimens to desired elevated temperatures for irradiation by a high energy neutron source. A furnace assembly is provided for heating two separate groups of specimens to substantially different, elevated, isothermal temperatures in a high vacuum environment while positioning the two specimen groups symmetrically at equivalent neutron irradiating positions.

  8. Furnace assembly

    DOEpatents

    Panayotou, N.F.; Green, D.R.; Price, L.S.

    A method of and apparatus for heating test specimens to desired elevated temperatures for irradiation by a high energy neutron source. A furnace assembly is provided for heating two separate groups of specimens to substantially different, elevated, isothermal temperatures in a high vacuum environment while positioning the two specimen groups symmetrically at equivalent neutron irradiating positions.

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

    USGS Publications Warehouse

    Jones, Sandra R.; Garbarino, John R.

    1999-01-01

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

  10. Levels of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and trace metals in the blood of nonoccupationally exposed residents living in the vicinity of a municipal solid waste incinerator and electric arc furnace.

    PubMed

    Chen, Yan-Min; Lin, Yuan-Chung; Wu, Tzi-Yi; Chang-Chien, Guo-Ping; Ma, Wen-Feng

    2010-06-01

    This study examines levels of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), and trace metals in the blood of the nonoccupationally exposed residents living in the vicinity of municipal solid waste incinerators (MSWIs) and electric arc furnaces (EAFs). The analysis found that older females had higher concentrations of PCDD/Fs and older males had higher body mass index (BMI) values and higher concentrations of PCDD/Fs. Moreover, sex appeared to affect the levels of PCDD/Fs because, overall, females showed higher levels of PCDD/Fs. The results of a principal component analysis indicated that the characteristics of the blood were more similar to the characteristics of the stack flux gas in MSWIs than those in EAFs. When sex, age, and BMI values were taken into consideration, none of the factors appeared to significantly affect PCDD/F and trace metal blood levels. However, when participants were divided into eight categories and analyzed, it was found that sex was the most important factor affecting levels of trace metals in blood and that males had higher concentrations of Pb, Al, Cd, and Cu.

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

    PubMed

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

    2016-10-01

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

  12. Laboratory experiments on arc deflection and instability

    SciTech Connect

    Zweben, S.; Karasik, M.

    2000-03-21

    This article describes experiments on arc deflection instability carried out during the past few years at the Princeton University Plasma Physics Laboratory (PPPL). The approach has been that of plasma physicists interested in arcs, but they believe these results may be useful to engineers who are responsible for controlling arc behavior in large electric steel furnaces.

  13. Graphite on graphite

    NASA Astrophysics Data System (ADS)

    Volovik, G. E.; Pudalov, V. M.

    2016-12-01

    We propose potential geometry for fabrication of the graphite sheets with atomically smooth edges. For such sheets with Bernal stacking, the electron-electron interaction and topology should cause sufficiently high density of states resulting in the high temperature of either spin ordering or superconducting pairing.

  14. 5. Photocopied August 1978. FRONT OF A HORRY ROTARY FURNACE, ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    5. Photocopied August 1978. FRONT OF A HORRY ROTARY FURNACE, SHOWING INTERIOR ELECTRODES. THE RAW MATERIALS FOR CALCIUM CARBIDE PRODUCTION--LIMESTONE AND COKE--WERE FED BY HOPPERS PLACED BETWEEN THESE ELECTRODES INTO THE ELECTRIC ARC. THE REMOVABLE PLATES ON THE EXTERNAL CIRCUMSTANCE OF THE HORRY FURNACE ARE SHOWN ON THE FIRST THREE FURNACES. (M) - Michigan Lake Superior Power Company, Portage Street, Sault Ste. Marie, Chippewa County, MI

  15. Emissions of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) from both of point and area sources of an electric-arc furnace-dust treatment plant and their impacts to the vicinity environments.

    PubMed

    Yu, Kuei-Min; Lee, Wen-Jhy; Tsai, Perng-Jy; Fang, Kenneth; Lin, Mark

    2010-08-01

    This study was set out to investigate emissions of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) from both the stack (i.e., point source) and plant fugitives (i.e., area source) of an electric-arc furnace-dust treatment plant (EAFDTP) and their impact to the vicinity environments. The emission rate of the point source (2,360 ng I-TEQh(-1)) was determined directly by measuring PCDD/F concentrations of the stack flue gas. The emission rate of the area source (1,080 ng I-TEQ m(-2)h(-1)) was estimated by using the Industrial Sources Complex Short-Term (ISCST3) model based on concentrations measured at the downwind side of the plant. The mean emission factors of 785 and 893 ng I-TEQ ton(-1) ZnO were found for the point and area source, respectively. The above results suggest that the area source accounted for more than 50% of total PCDD/F emissions for the selected EAFDTP. The contribution of the point source to the atmospheric PCDD/F concentrations of the upwind site and downwind site of the EAFDTP were 0 and 0.27 fg I-TEQ Nm(-3), respectively. The contributions of the area source were 0.020 and 3.3 fg I-TEQ Nm(-3), respectively. The total contribution of the selected EAFDTP (including both the point and area sources) to the concentrations in both upwind and downwind side vicinities were all less than 10%. Finally, the impact of PCDD/F emissions from the selected EAFDTP to the vicinity atmospheric environments was discussed in the present study.

  16. Maintaining vacuum furnaces

    SciTech Connect

    Kowalewski, J.

    2000-04-01

    A preventive maintenance program is essential for safe and consistent vacuum furnace operation. The program should be developed in cooperation with safety, maintenance, and furnace operators, implemented as soon as the furnace is commissioned, and adhered to throughout the life of the furnace. This article serves as an introduction to the topic of vacuum furnace preventive maintenance. Basic information about installing a new vacuum furnace also is provided.

  17. Radiation heat transfer within an optical fiber draw tower furnace

    SciTech Connect

    Issa, J.; Jaluria, Y.; Polymeropoulos, C.E.; Yin, Z.

    1995-12-31

    Study of the thermal transport and material flow processes associated with the drawing of optical fiber in a graphite draw furnace requires modeling of the heat transfer from the furnace wall. Previous work has shown that accurate knowledge of the furnace heater element axial temperature distribution is essential for proper modeling of the radiative transfer process. The present work is aimed at providing this information, as well as generating a set of data for the study of radiation exchange in the furnace cavity. The experimental procedure involved measuring the centerline temperature distribution in graphite and fused silica rods inserted into an optical fiber draw tower furnace. The temperature measurements were then used along with a model for radiative-convective heat transfer in the furnace in order to obtain the furnace temperature profile. This is an inverse problem since the centerline temperature in the rod is known whereas the furnace thermal conditions are not. The results obtained showed that the furnace temperature distribution was independent of rod material and size. The shape of the computed temperature distributions suggest that they can be well represented by a Gaussian function.

  18. High temperature aircraft research furnace facilities

    NASA Technical Reports Server (NTRS)

    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.

  19. Industrial furnace

    SciTech Connect

    Shostak, V.M.; Tolochko, A.I.; Volkov, V.P.; Maradudin, G.I.; Schekin, N.G.; Popov, M.I.; Shepelev, D.N.; Matveev, A.I.; Butnyakov, A.I.; Rzhavichev, A.P.

    1986-09-02

    An industrial furnace is described which consists of: a bath made of a refractory material for filling with a melt; a direct current source; main current-carrying elements having free ends extending to an operating area of the refractory material of the bath below and above the melt, and the main current-carrying elements extending to the operating area below the melt being connected with opposite terminals of the current source from the main current-carrying elements extending to the operating area above the melt; and additional current-carrying elements having free ends sunk in the refractory material of the bath below and above the melt and the additional current-carrying elements being connected with the terminals of the power source of opposite polarity with respect to the connection of the main current-carrying elements of a corresponding part of the operating area.

  20. Designing modern furnace cooling systems

    NASA Astrophysics Data System (ADS)

    Merry, J.; Sarvinis, J.; Voermann, N.

    2000-02-01

    An integrated multidisciplinary approach to furnace design that considers the interdependence between furnace cooling elements and other furnace systems, such as binding, cooling water, and instrumentation, is necessary to achieve maximum furnace production and a long refractory life. The retrofit of the BHP Hartley electric furnace and the Kidd Creek copper converting furnace are successful examples of an integrated approach to furnace cooling design.

  1. Graphite-Fiber-Reinforced Glass-Matrix Composite

    NASA Technical Reports Server (NTRS)

    Prewo, K. M.; Dicus, D. L.

    1982-01-01

    G/GI structural composite material made of graphite fibers embedded in borosilicate glass exhibit excellent strength, fracture toughness, and dimensional stability at elevated temperatures. It is made by passing graphite-fiber yarn through slurry containing suspension of fine glass particles in carrier liquid and winding on drum to produce prepegged uniaxial tape. After drying, tapes are cut into appropriate lengths and laid up in graphite die in desired stacking scheme. Stack is consolidated by hot pressing in furnace.

  2. GRAPHITE EXTRUSIONS

    DOEpatents

    Benziger, T.M.

    1959-01-20

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

  3. Unstable behavior of anodic arc discharge for synthesis of nanomaterials

    DOE PAGES

    Gershman, Sophia; Raitses, Yevgeny

    2016-07-27

    A short carbon arc operating with a high ablation rate of the graphite anode exhibits a combined motion of the arc and the arc attachment to the anode. A characteristic time scale of this motion is in a 10-3 sec range. The arc exhibits a negative differential resistance before the arc motion occurs. Thermal processes in the arc plasma region interacting with the ablating anode are considered as possible causes of this unstable arc behavior. It is also hypothesized that the arc motion could potentially cause mixing of the various nanoparticles synthesized in the arc in the high ablation regime.

  4. Unstable behavior of anodic arc discharge for synthesis of nanomaterials

    SciTech Connect

    Gershman, Sophia; Raitses, Yevgeny

    2016-07-27

    A short carbon arc operating with a high ablation rate of the graphite anode exhibits a combined motion of the arc and the arc attachment to the anode. A characteristic time scale of this motion is in a 10-3 sec range. The arc exhibits a negative differential resistance before the arc motion occurs. Thermal processes in the arc plasma region interacting with the ablating anode are considered as possible causes of this unstable arc behavior. It is also hypothesized that the arc motion could potentially cause mixing of the various nanoparticles synthesized in the arc in the high ablation regime.

  5. Unstable behavior of anodic arc discharge for synthesis of nanomaterials

    SciTech Connect

    Gershman, Sophia; Raitses, Yevgeny

    2016-07-27

    A short carbon arc operating with a high ablation rate of the graphite anode exhibits a combined motion of the arc and the arc attachment to the anode. A characteristic time scale of this motion is in a 10-3 sec range. The arc exhibits a negative differential resistance before the arc motion occurs. Thermal processes in the arc plasma region interacting with the ablating anode are considered as possible causes of this unstable arc behavior. It is also hypothesized that the arc motion could potentially cause mixing of the various nanoparticles synthesized in the arc in the high ablation regime.

  6. Arc initiation in cathodic arc plasma sources

    SciTech Connect

    Anders, Andre

    2002-01-01

    A "triggerless" arc initiation method and apparatus is based on simply switching the arc supply voltage to the electrodes (anode and cathode). Neither a mechanical trigger electrode nor a high voltage flashover from a trigger electrode is required. A conducting path between the anode and cathode is provided, which allows a hot spot to form at a location where the path connects to the cathode. While the conductive path is eroded by the cathode spot action, plasma deposition ensures the ongoing repair of the conducting path. Arc initiation is achieved by simply applying the relatively low voltage of the arc power supply, e.g. 500 V-1 kV, with the insulator between the anode and cathode coated with a conducting layer and the current at the layer-cathode interface concentrated at one or a few contact points. The local power density at these contact points is sufficient for plasma production and thus arc initiation. A conductive surface layer, such as graphite or the material being deposited, is formed on the surface of the insulator which separates the cathode from the anode. The mechanism of plasma production (and arc initiation) is based on explosive destruction of the layer-cathode interface caused by joule heating. The current flow between the thin insulator coating and cathode occurs at only a few contact points so the current density is high.

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

    PubMed

    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.

  8. Arc Distribution During the Vacuum Arc Remelting of Ti-6Al-4V

    NASA Astrophysics Data System (ADS)

    Woodside, C. Rigel; King, Paul E.; Nordlund, Chris

    2013-02-01

    Currently, the temporal distribution of electric arcs across the ingot during vacuum arc remelting (VAR) is not a known or monitored process parameter. Previous studies indicate that the distribution of arcs can be neither diffuse nor axisymmetric about the center of the furnace. Correct accounting for the heat flux, electric current flux, and mass flux into the ingot is critical to achieving realistic solidification models of the VAR process. The National Energy Technology Laboratory has developed an arc position measurement system capable of locating arcs and determining the arc distribution within an industrial VAR furnace. The system is based on noninvasive magnetic field measurements and a VAR specific form of the Biot-Savart law. The system was installed on a coaxial industrial VAR furnace at ATI Albany Operations in Albany, OR. This article reports on the different arc distributions observed during production of Ti-6Al-4V. It is shown that several characteristic arc distribution modes can develop. This behavior is not apparent in the existing signals used to control the furnace, indicating the measurement system is providing new information. It is also shown that the different arc distribution modes observed may impact local solidification times, particularly at the side wall.

  9. Arc distribution during the vacuum arc remelting of Ti-6Al-4V

    SciTech Connect

    Woodside, Charles Rigel; King, Paul E.; Nordlund, Chris

    2013-01-01

    Currently, the temporal distribution of electric arcs across the ingot during vacuum arc remelting (VAR) is not a known or monitored process parameter. Previous studies indicate that the distribution of arcs can be neither diffuse nor axisymmetric about the center of the furnace. Correct accounting for the heat flux, electric current flux, and mass flux into the ingot is critical to achieving realistic solidification models of the VAR process. The National Energy Technology Laboratory has developed an arc position measurement system capable of locating arcs and determining the arc distribution within an industrial VAR furnace. The system is based on noninvasive magnetic field measurements and a VAR specific form of the Biot–Savart law. The system was installed on a coaxial industrial VAR furnace at ATI Albany Operations in Albany, OR. This article reports on the different arc distributions observed during production of Ti-6Al-4V. It is shown that several characteristic arc distribution modes can develop. This behavior is not apparent in the existing signals used to control the furnace, indicating the measurement system is providing new information. It is also shown that the different arc distribution modes observed may impact local solidification times, particularly at the side wall.

  10. Paired Straight Hearth Furnace - Transformational Ironmaking Process

    SciTech Connect

    Lu, Wei-Kao; Debski, Paul

    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.

  11. Heat treatment furnace

    DOEpatents

    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.

  12. Graphite Formation in Cast Iron

    NASA Technical Reports Server (NTRS)

    Stefanescu, D. M.

    1985-01-01

    In the first phase of the project it was proven that by changing the ratio between the thermal gradient and the growth rate for commercial cast iron samples solidifying in a Bridgman type furnace, it is possible to produce all types of graphite structures, from flake to spheroidal, and all types of matrices, from ferritic to white at a certain given level of cerium. KC-135 flight experiments have shown that in a low-gravity environment, no flotation occurs even in spheroidal graphite cast irons with carbon equivalent as high as 5%, while extensive graphite flotation occurred in both flake and spheroidal graphite cast irons, in high carbon samples solidified in a high gravity environment. This opens the way for production of iron-carbon composite materials, with high carbon content (e.g., 10%) in a low gravity environment. By using KC-135 flights, the influence of some basic elements on the solidification of cast iron will be studied. The mechanism of flake to spheroidal graphite transition will be studied, by using quenching experiments at both low and one gravity for different G/R ratios.

  13. 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.

    PubMed

    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 < HO(4)Q < HO(6)Q. The 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.

  14. A fast and accurate method for the determination of total and soluble fluorine in toothpaste using high-resolution graphite furnace molecular absorption spectrometry and its comparison with established techniques.

    PubMed

    Gleisner, Heike; Einax, Jürgen W; Morés, Silvane; Welz, Bernhard; Carasek, Eduardo

    2011-04-05

    A fast and reliable method has been developed for the determination of total and soluble fluorine in toothpaste, important quality control parameters in dentifrices. The method is based on the molecular absorption of gallium mono-fluoride, GaF, using a commercially available high-resolution continuum source atomic absorption spectrometer. Transversely heated platform tubes with zirconium as permanent chemical modifier were used throughout. Before each sample injection, a palladium and zirconium modifier solution and a gallium reagent were deposited onto the graphite platform and thermally pretreated to transform them into their active forms. The samples were only diluted and introduced directly into the graphite tube together with additional gallium reagent. Under these conditions the fluoride was stable up to a pyrolysis temperature of 550 °C, and the optimum vaporization (molecule formation) temperature was 1550 °C. The GaF molecular absorption was measured at 211.248 nm, and the limits of detection and quantification were 5.2 pg and 17 pg, respectively, corresponding to a limit of quantification of about 30 μg g(-1) (ppm) F in the original toothpaste. The proposed method was used for the determination of total and soluble fluorine content in toothpaste samples from different manufactures. The samples contained different ionic fluoride species and sodium monofluorophosphate (MFP) with covalently bonded fluorine. The results for total fluorine were compared with those obtained with a modified conventional headspace gas chromatographic procedure. Accuracy and precision of the two procedures were comparable, but the proposed procedure was much less labor-intensive, and about five times faster than the latter one. Copyright © 2010 Elsevier B.V. All rights reserved.

  15. Graphite Revisited

    NASA Astrophysics Data System (ADS)

    Draine, B. T.

    2016-11-01

    Laboratory measurements are used to constrain the dielectric tensor for graphite, from microwave to X-ray frequencies. The dielectric tensor is strongly anisotropic even at X-ray energies. The discrete dipole approximation is employed for accurate calculations of absorption and scattering by single-crystal graphite spheres and spheroids. For randomly oriented single-crystal grains, the so-called 1/3{--}2/3 approximation for calculating absorption and scattering cross sections is exact in the limit a/λ \\to 0 and provides better than ∼10% accuracy in the optical and UV even when a/λ is not small, but becomes increasingly inaccurate at infrared wavelengths, with errors as large as ∼40% at λ =10 μ {{m}}. For turbostratic graphite grains, the Bruggeman and Maxwell Garnett treatments yield similar cross sections in the optical and ultraviolet, but diverge in the infrared, with predicted cross sections differing by over an order of magnitude in the far-infrared. It is argued that the Maxwell Garnett estimate is likely to be more realistic, and is recommended. The out-of-plane lattice resonance of graphite near 11.5 μm may be observable in absorption with the MIRI spectrograph on James Webb Space Telescope. Aligned graphite grains, if present in the interstellar medium, could produce polarized X-ray absorption and polarized X-ray scattering near the carbon K edge.

  16. Electromelt furnace evaluation

    SciTech Connect

    Reimann, G.A.; Welch, J.M.

    1981-09-01

    An electromelt furnace was designed, built, and operated at the Idaho National Engineering Laboratory to demonstrate the suitability of this equipment for large-scale processing of radioactive wastes in iron-enriched basalt. Several typical waste compositions were melted and cast. The furnace was disassembled and the components evaluated. Calcines and fluorides attacked the furnace lining, unoxidized metals accumulated under the slag, and electrode attrition was high.

  17. Electromelt furnace evaluation

    NASA Astrophysics Data System (ADS)

    Reimann, G. A.; Welch, J. M.

    1981-09-01

    An electromelt furnace was designed, built and operated at the Idaho National Engineering Laboratory to demonstrate the suitability of this equipment for large-scale processing of radioactive wastes in iron-enriched basalt. Several typical waste compositions were melted and cast. The furnace was disassembled and the components evaluated. Calcines and fluorides attacked the furnace lining, unoxidized metals accumulated under the slag, and electrode attrition was high.

  18. EXTERIOR VIEW, BLAST FURNACE NO. 3 (JANE FURNACE) CENTER, NO. ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    EXTERIOR VIEW, BLAST FURNACE NO. 3 (JANE FURNACE) CENTER, NO. 3 CAST HOUSE TO THE LEFT, WEST ORE BRIDGE TO THE RIGHT. - Pittsburgh Steel Company, Monessen Works, Blast Furnace No. 3, Donner Avenue, Monessen, Westmoreland County, PA

  19. Advanced steel reheat furnace

    SciTech Connect

    Moyeda, D.; Sheldon, M.; Koppang, R.; Lanyi, M.; Li, X.; Eleazer, B.

    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.

  20. General view of blast furnace plant, with blast furnace "A" ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    General view of blast furnace plant, with blast furnace "A" (built in 1907) to the left; in the foreground is the turbo-blower and blast furnace gas-powered electric generating station (built in 1919), looking northwest - Bethlehem Steel Corporation, South Bethlehem Works, Blast Furnace "A", Along Lehigh River, North of Fourth Street, West of Minsi Trail Bridge, Bethlehem, Northampton County, PA

  1. INTERIOR VIEW SHOWING FURNACE KEEPER OBSERVING FURNACE THROUGH BLUE GLASS ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    INTERIOR VIEW SHOWING FURNACE KEEPER OBSERVING FURNACE THROUGH BLUE GLASS EVERY TWENTY MINUTES TO DETERMINE SIZE AND TEXTURE OF BATCH AND OTHER VARIABLES. FAN IN FRONT COOLS WORKERS AS THEY CONDUCT REPAIRS. FURNACE TEMPERATURE AT 1572 DEGREES FAHRENHEIT. - Chambers-McKee Window Glass Company, Furnace No. 2, Clay Avenue Extension, Jeannette, Westmoreland County, PA

  2. General purpose rocket furnace

    NASA Technical Reports Server (NTRS)

    Aldrich, B. R.; Whitt, W. D. (Inventor)

    1979-01-01

    A multipurpose furnace for space vehicles used for material processing experiments in an outer space environment is described. The furnace contains three separate cavities designed to process samples of the widest possible range of materials and thermal requirements. Each cavity contains three heating elements capable of independent function under the direction of an automatic and programmable control system. A heat removable mechanism is also provided for each cavity which operates in conjunction with the control system for establishing an isothermally heated cavity or a wide range of thermal gradients and cool down rates. A monitoring system compatible with the rocket telemetry provides furnace performance and sample growth rate data throughout the processing cycle.

  3. High Temperature Transparent Furnace Development

    NASA Technical Reports Server (NTRS)

    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.

  4. Refractory Corrosion Mechanisms in a Novel High Carbon Ferromanganese Production Furnace

    NASA Astrophysics Data System (ADS)

    Gregurek, D.; Wenzl, C.; Kreuzer, D.; Spanring, A.; Kirschen, M.; Zeelie, D.; Groenewald, J.

    2016-12-01

    The present paper presents the refractory design for a novel HCFeMn smelting furnace that, other than standard submerged arc furnaces, allows the processing of fine ores. A combination of basic and non-basic materials, comprising bricks, castables and ramming was chosen, under consideration of the unique furnace design and process conditions. Post-mortem investigations on refractory samples from the different furnace zones were carried out and provided information about the main wear mechanism. Additionally, investigations of the process slag and metal were carried out both practically and theoretically using thermodynamic calculations, to better understand the corrosion phenomena observed in the post mortem samples.

  5. Thermally exfoliated graphite oxide

    NASA Technical Reports Server (NTRS)

    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. Paired Straight Hearth Furnace

    SciTech Connect

    2009-04-01

    This factsheet describes a research project whose goals are to design, develop, and evaluate the scalability and commercial feasibility of the PSH Paired Straight Hearth Furnace alternative ironmaking process.

  7. Commercial Float Zone Furnace

    NASA Image and Video Library

    1996-05-25

    S77-E-5094 (25 May 1996) --- Astronaut Marc Garneau, mission specialist representing the Canadian Space Agency (CSA), stands at the Commercial Float Zone Furnace (CFZF) in the Spacehab Module onboard the Earth-orbiting Space Shuttle Endeavour.

  8. Space Station Furnace Facility

    SciTech Connect

    Cobb, S.D.; Lehoczky, S.L.

    1996-12-31

    The Space Station Furnace Facility (SSFF) is the modular, multi-user scientific instrumentation for conducting materials research in the reduced gravity ({approximately}10{sup {minus}6} g) environment of the International Space Station (ISS). The facility is divided into the Core System and two Instrument Racks (IRs). The Core System provides the common electrical and mechanical support equipment required to operate Experiment Modules (EMs). The EMs are investigator unique furnaces or apparatus designed to accomplish specific science investigations. Investigations are peer selected every two years from proposals submitted in response to National Aeronautics and Space Administration (NASA) Research Announcements. The SSFF Core systems are designed to accommodate an envelope of eight types of experiment modules. The first two modules to be developed for the first Instrument Rack include a High Temperature Gradient Furnace with Quench (HGFQ), and a Low Temperature Gradient Furnace (LGF). A new EM is planned to be developed every two years.

  9. Durable cathodes for high-power inert-gas arcs

    NASA Technical Reports Server (NTRS)

    Decker, A. J.; Gettleman, C. C.; Goldman, G. C.; Hall, J. H.; Pollack, J. L.

    1971-01-01

    Cathode design minimizes evaporation of electrode material which may deposit on associated optical surfaces. It also results in stable operation and precise positioning of arc relative to optical collector. Innovation applies to high power light sources and to arcs used in industrial furnaces.

  10. High temperature furnace

    DOEpatents

    Borkowski, Casimer J.

    1976-08-03

    A high temperature furnace for use above 2000.degree.C is provided that features fast initial heating and low power consumption at the operating temperature. The cathode is initially heated by joule heating followed by electron emission heating at the operating temperature. The cathode is designed for routine large temperature excursions without being subjected to high thermal stresses. A further characteristic of the device is the elimination of any ceramic components from the high temperature zone of the furnace.

  11. Bridged graphite oxide materials

    NASA Technical Reports Server (NTRS)

    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.

  12. Nuclear graphite

    SciTech Connect

    Mercuri, R. A.; Criscione, J. M.

    1985-07-02

    A high strength, high coefficient of thermal expansion fine-grained isotropic graphite article produced from 30% to 70% of attritor milled gilsonite coke or other high CTE carbon filler particles and minor amounts of a binder such a coal tar pitch and petroleum pitch, the article being formed by warm isostatic molding at a temperature of between 50/sup 0/ C. and 70/sup 0/ C. under a pressure between 100 and 1000 psi for a time between 1 and 10 minutes. The particle size of the fillers ranges up to 150 microns.

  13. Effects of furnace pressure on oxygen and carbon coupled transport in an industrial directional solidification furnace for crystalline silicon ingots

    NASA Astrophysics Data System (ADS)

    Qi, Xiaofang; Liu, Lijun; Ma, Wencheng

    2017-06-01

    Transient global simulations were carried out to study the effects of the furnace pressure on oxygen (O) and carbon (C) coupled transport in an industrial directional solidification (DS) furnace for silicon ingots. The global simulations of impurity transport, taking into account the O and C impurity segregation, chemical reaction on the graphite surface, evaporation of SiO and dissolution of CO at the melt-gas surface, were based on a fully coupled calculation of the thermal and flow fields of the DS furnace. It was found that the furnace pressure affects the intensity and structure of argon flow above the melt surface, which further influences the O and C impurities transport in the DS furnace. The O concentration in the grown ingot decreases with the decreasing furnace pressure. While the C concentration first decreases, and then increases when the pressure is smaller than 200 mbar due to the strong diffusion effect of the CO through the gap between crucible and cover. The numerical predictions of O and C concentrations agree well with the experimental measurements.

  14. High gradient directional solidification furnace

    NASA Technical Reports Server (NTRS)

    Aldrich, B. R.; Whitt, W. D. (Inventor)

    1985-01-01

    A high gradient directional solidification furnace is disclosed which includes eight thermal zones throughout the length of the furnace. In the hot end of the furnace, furnace elements provide desired temperatures. These elements include Nichrome wire received in a grooved tube which is encapsulated y an outer alumina core. A booster heater is provided in the hot end of the furnace which includes toroidal tungsten/rhenium wire which has a capacity to put heat quickly into the furnace. An adiabatic zone is provided by an insulation barrier to separate the hot end of the furnace from the cold end. The old end of the furnace is defined by additional heating elements. A heat transfer plate provides a means by which heat may be extracted from the furnace and conducted away through liquid cooled jackets. By varying the input of heat via the booster heater and output of heat via the heat transfer plate, a desired thermal gradient profile may be provided.

  15. Better VPS Fabrication of Crucibles and Furnace Cartridges

    NASA Technical Reports Server (NTRS)

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

    2003-01-01

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

  16. Blast furnaces make way for new steel technology

    SciTech Connect

    Ondrey, G.; Parkinson, G.; Moore, S.

    1995-03-01

    Increasingly stringent environmental regulations, aging production units, and a competitive market are forcing iron and steelmakers to improve the environmental performance and cost efficiencies of their processes. The traditional integrated steel unit isn`t obsolete -- yet. Blast furnaces will be around for at least another 15 years. However, traditional technology is in for some changes, and stepped up rivalry from electric arc furnace minimills and ironmaking processes that use gas or coal. The paper discusses direct iron making processes, the DRI-minimill connection, the iron carbide process, and reclaiming iron from waste.

  17. Looking Northwest at Furnace Control Panels and Gas Control Furnace ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    Looking Northwest at Furnace Control Panels and Gas Control Furnace in Red Room Within Recycle Recovery Building - Hematite Fuel Fabrication Facility, Recycle Recovery Building, 3300 State Road P, Festus, Jefferson County, MO

  18. Monitoring lining and hearth conditions at Inland`s No. 7 blast furnace

    SciTech Connect

    Quisenberry, P.; Grant, M.; Carter, W.

    1997-12-31

    The paper describes: furnace statistics; mini-reline undertaken in November, 1993; the stack condition; throat gunning; stabilizing the graphite bricks; the hearth condition; reactions to temperature excursions; future instrumentation; and hot blast system areas of concern. The present data from monitoring systems and inspections indicate that the furnace should be able to operate well beyond the expectation for the 1993 mini-reline (3--5 years) with: (1) consistent, high quality raw materials; (2) instrumentation, diagnostic, remedial, and preventative techniques developed; and (3) stopping quickly any water leaks into the furnace. The longevity of this campaign has undoubtedly been a result of this monitoring program.

  19. Regularities of heat transfer in the gas layers of a steam boiler furnace flame. Part II. Gas layer radiation laws and the procedure for calculating heat transfer in furnaces, fire boxes, and combustion chambers developed on the basis of these laws

    NASA Astrophysics Data System (ADS)

    Makarov, A. N.

    2014-10-01

    The article presents the results stemming from the scientific discovery of laws relating to radiation from the gas layers generated during flame combustion of fuel and when electric arc burns in electric-arc steel-melting furnaces. The procedure for calculating heat transfer in electric-arc and torch furnaces, fire-boxes, and combustion chambers elaborated on the basis of this discovery is described.

  20. Preparation of graphitic articles

    DOEpatents

    Phillips, Jonathan; Nemer, Martin; Weigle, John C.

    2010-05-11

    Graphitic structures have been prepared by exposing templates (metal, metal-coated ceramic, graphite, for example) to a gaseous mixture that includes hydrocarbons and oxygen. When the template is metal, subsequent acid treatment removes the metal to yield monoliths, hollow graphitic structures, and other products. The shapes of the coated and hollow graphitic structures mimic the shapes of the templates.

  1. An improved gas extraction furnace

    NASA Technical Reports Server (NTRS)

    Wilkin, R. B.

    1972-01-01

    Design of glass furnace for analysis of rocks to determine nature and amount of trapped gas is described. Furnace heats specimen in vacuum conditions by radio frequency induction. Diagram of apparatus to show construction and operation is provided.

  2. Cathodic arcs

    SciTech Connect

    Anders, Andre

    2003-10-29

    Cathodic arc plasma deposition has become the technology of choice for hard, wear and corrosion resistant coatings for a variety of applications. The history, basic physics of cathodic arc operation, the infamous macroparticle problem and common filter solutions, and emerging high-tech applications are briefly reviewed. Cathodic arc plasmas standout due to their high degree of ionization, with important consequences for film nucleation, growth, and efficient utilization of substrate bias. Industrial processes often use cathodic arc plasma in reactive mode. In contrast, the science of arcs has focused on the case of vacuum arcs. Future research directions include closing the knowledge gap for reactive mode, large area coating, linear sources and filters, metal plasma immersion process, with application in high-tech and biomedical fields.

  3. Carbon rod furnace infrared source

    NASA Technical Reports Server (NTRS)

    Boyd, W. J.; Jennings, D. E.; Blass, W. E.; Gailar, N. M.

    1974-01-01

    A carbon rod furnace infrared source has been built and has proven to be a reliable and trouble-free source despite the high rod temperature of 2500 K. The furnace offers several advantages over previous furnaces. These include an increase in usable rod length to 6.35 cm, extended rod life, and a fully automated power supply for the furnace. Construction and operational details are discussed.

  4. CHARGING SIDE OF #130 ELECTRIC FURNACE CO. REHEAT FURNACE IN ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    CHARGING SIDE OF #130 ELECTRIC FURNACE CO. REHEAT FURNACE IN REROLL BAY. CAKES FROM THE CASTING SHOP ARE BROUGHT UP TO ROLLING TEMPERATURE IN ONE OF TWO (#130 AND 146) GAS-FIRED FURNACES. A RADIO-CONTROLLED OVERHEAD CRANE TRANSFERS CAKES FROM FLATCARS TO THE ROLLER LINE LEADING INTO THE FURNACE. CAKES ARE HEATED AT 900-1000 DEGREES FAHRENHEIT FOR THREE TO FOUR HOURS. RATED FURNACE CAPACITY IS 100,000 LBS.\\HOUR. - American Brass Foundry, 70 Sayre Street, Buffalo, Erie County, NY

  5. Commercial Float Zone Furnace

    NASA Image and Video Library

    1996-05-25

    S77-E-5093 (25 May 1996) --- Astronaut Marc Garneau, mission specialist representing the Canadian Space Agency (CSA), makes a visual check of the Commercial Float Zone Furnace (CFZF), a single-rack-mounted facility in the Spacehab Module onboard the Earth-orbiting Space Shuttle Endeavour. The scene was recorded with an Electronic Still Camera (ESC).

  6. Strengthen flame stability during the furnace`s load decrease

    SciTech Connect

    Zhang Zhiguo; Sun Xuexin; Li Fujin; Qiu Jihua; Chen Gang

    1996-12-31

    This paper presents the result of the study of the coal combustion characteristic and flame stability during the load decrease of PCFF (corner burner arrangement). Considering the relation between flame stability and furnace load during the furnace load change, some method must be used to strengthen the pulverized coal ignition and combustion for the furnace to maintain the flame stability especially for the furnace which fires low rank anthracite. Experimental results show that when the furnace load decreased, the temperature distribution in furnace decreased and the flame stability in furnace had changed because of the load changing. This paper also introduces a new pulverized coal burner: Bluff-body with cavity burner. According to the result of application of this burner, this kind of pulverized coal burner can improve the coal ignition and combustion efficiency. Especially for low load operation of furnace the bluff-body with cavity burner has demonstrated its ability in strengthening coal ignition and improving the flame stability for furnace operation. Experimental results show that using bluff-body with cavity burner, the lowest load for furnace fired bituminous is 40% MCR and 50% MCr for low rank anthracite (V{sup r} < 12%, A{sup f} > 45%). This burner has simple structure and is very easy to set up for furnace.

  7. Controlling electrode gap during vacuum arc remelting at low melting current

    DOEpatents

    Williamson, R.L.; Zanner, F.J.; Grose, S.M.

    1997-04-15

    An apparatus and method are disclosed for controlling electrode gap in a vacuum arc remelting furnace, particularly at low melting currents. Spectrographic analysis is performed of the metal vapor plasma, from which estimates of electrode gap are derived. 5 figs.

  8. Controlling electrode gap during vacuum arc remelting at low melting current

    DOEpatents

    Williamson, Rodney L.; Zanner, Frank J.; Grose, Stephen M.

    1997-01-01

    An apparatus and method for controlling electrode gap in a vacuum arc remelting furnace, particularly at low melting currents. Spectrographic analysis is performed of the metal vapor plasma, from which estimates of electrode gap are derived.

  9. Status of Graphite Oxidation Work

    SciTech Connect

    Rebecca Smith

    2010-05-01

    Data were developed to compare the extent of structural damage associated with high temperature exposure to an air leak. Two materials, NBG-18 graphite and unpurified PCEA graphite have been tested as of this report. The scope was limited to isothermal oxidation at a single temperature, 750°C. Ambient post-oxidation compression strength testing was performed for three levels of burn off (1%, 5%, and 10% mass loss) for two leak scenarios: 100% air and 10% air in helium. Temperature, gas flow, and dynamic mass loss oxidation conditions were monitored and recorded for each sample. The oxidation period was controlled with flow of inert gas during the thermal ramp and upon cool down with a constant 10 liter per minute flow maintained throughout furnace operation. Compressive strengths of parallel un-oxidized samples were tested to assess the relative mass loss effects. In addition to baseline samples matching the un-oxidized dimensions of the oxidized samples, two sets of mechanically reduced samples were prepared. One set was trimmed to achieve the desired mass loss by removing an effectively uniform depth from the geometric surface of the sample. The other set was cored to produce a full penetration axial hole down the center of each sample.

  10. Calculation of the Temperature Drop for High-Temperature Fixed Points for Different Furnace Conditions

    NASA Astrophysics Data System (ADS)

    Castro, P.; Machin, G.; Villamañan, M. A.; Lowe, D.

    2011-08-01

    High-temperature fixed points (HTFPs) based on eutectic and peritectic reactions of metals and carbon are likely to become, in the near term, reference standards at high temperatures. Typically for radiation thermometry applications, these HTFPs are generally formed of a graphite crucible, with a reentrant well, an included 120° cone, and a nominal aperture of 3 mm. It is important to quantify the temperature drop at the back wall of the cavity, and to understand the influence of the crucible configuration and furnace conditions on this drop. In order to study these influences, three different situations have been modeled by means of the finite volume method for numerical analysis. The first investigates the influence of the furnace temperature profile on the temperature drop by simulating four different furnace conditions. The other two study variations in the crucible configuration, namely, the thickness of the graphite back wall and the length of the blackbody tube.

  11. Electric-arc synthesis of soot with high content of higher fullerenes in parallel arc

    NASA Astrophysics Data System (ADS)

    Dutlov, A. E.; Nekrasov, V. M.; Sergeev, A. G.; Bubnov, V. P.; Kareev, I. E.

    2016-12-01

    Soot with a relatively high content of higher fullerenes (C76, C78, C80, C82, C84, C86, etc.) is synthesized in a parallel arc upon evaporation of pure carbon electrodes. The content of higher fullerenes in soot extract amounts to 13.8 wt % when two electrodes are simultaneously burnt in electric-arc reactor. Such a content is comparable with the content obtained upon evaporation of composite graphite electrodes with potassium carbonate impurity.

  12. Chapter 20: Graphite

    SciTech Connect

    Burchell, Timothy D

    2012-01-01

    Graphite is truly a unique material. Its structure, from the nano- to the millimeter scale give it remarkable properties that lead to numerous and diverse applications. Graphite bond anisotropy, with strong in-plane covalent bonds and weak van der Waals type bonding between the planes, gives graphite its unique combination of properties. Easy shear of the crystal, facilitated by weak interplaner bonds allows graphite to be used as a dry lubricant, and is responsible for the substances name! The word graphite is derived from the Greek to write because of graphites ability to mark writing surfaces. Moreover, synthetic graphite contains within its structure, porosity spanning many orders of magnitude in size. The thermal closure of these pores profoundly affects the properties for example, graphite strength increases with temperature to temperatures in excess of 2200 C. Consequently, graphite is utilized in many high temperature applications. The basic physical properties of graphite are reviewed here. Graphite applications include metallurgical; (aluminum and steel production), single crystal silicon production, and metal casting; electrical (motor brushes and commutators); mechanical (seals, bearings and bushings); and nuclear applications, (see Chapter 91, Nuclear Graphite). Here we discuss the structure, manufacture, properties, and applications of Graphite.

  13. Mercury in dumped blast furnace sludge.

    PubMed

    Földi, Corinna; Dohrmann, Reiner; Mansfeldt, Tim

    2014-03-01

    Blast furnace sludge (BFS) is a waste generated in the production of pig iron and was dumped in sedimentation ponds. Sixty-five samples from seven BFS locations in Europe were investigated regarding the toxic element mercury (Hg) for the first time. The charge material of the blast furnace operations revealed Hg contents from 0.015 to 0.097mgkg(-1). In comparison, the Hg content of BFS varied between 0.006 and 20.8mgkg(-1) with a median of 1.63mgkg(-1), which indicates enrichment with Hg. For one site with a larger sample set (n=31), Hg showed a stronger correlation with the total non-calcareous carbon (C) including coke and graphite (r=0.695; n=31; p<0.001). It can be assumed that these C-rich compounds are hosting phases for Hg. The solubility of Hg was rather low and did not exceed 0.43% of total Hg. The correlation between the total Hg concentration and total amount of NH4NO3-soluble Hg was relatively poor (r=0.496; n=27; p=0.008) indicating varying hazard potentials of the different BFS. Finally, BFS is a mercury-containing waste and dumped BFS should be regarded as potentially mercury-contaminated sites. Copyright © 2013 Elsevier Ltd. All rights reserved.

  14. Graphite filter atomizer in atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Katskov, Dmitri A.

    2007-09-01

    Graphite filter atomizers (GFA) for electrothermal atomic absorption spectrometry (ETAAS) show substantial advantages over commonly employed electrothermal vaporizers and atomizers, tube and platform furnaces, for direct determination of high and medium volatility elements in matrices associated with strong spectral and chemical interferences. Two factors provide lower limits of detection and shorter determination cycles with the GFA: the vaporization area in the GFA is separated from the absorption volume by a porous graphite partition; the sample is distributed over a large surface of a collector in the vaporization area. These factors convert the GFA into an efficient chemical reactor. The research concerning the GFA concept, technique and analytical methodology, carried out mainly in the author's laboratory in Russia and South Africa, is reviewed. Examples of analytical applications of the GFA in AAS for analysis of organic liquids and slurries, bio-samples and food products are given. Future prospects for the GFA are discussed in connection with analyses by fast multi-element AAS.

  15. Blast furnace stove control

    SciTech Connect

    Muske, K.R.; Hansen, G.A.; Howse, J.W.; Cagliostro, D.J.; Chaubal, P.C.

    1998-12-31

    This paper outlines the process model and model-based control techniques implemented on the hot blast stoves for the No. 7 Blast Furnace at the Inland Steel facility in East Chicago, Indiana. A detailed heat transfer model of the stoves is developed. It is then used as part of a predictive control scheme to determine the minimum amount of fuel necessary to achieve the blast air requirements. The controller also considers maximum and minimum temperature constraints within the stove.

  16. The investigation of carbon nitride films prepared at various arc currents by vacuum cathode arc method

    NASA Astrophysics Data System (ADS)

    Zhou, Zhimin; Xia, Lifang

    2002-08-01

    The carbon nitride films have been prepared in the arc currents range of 20-60 A at the Ar/N2 atmosphere of 50/400 sccm by the vacuum cathode arc deposition method. The properties of the films were characterized by x-ray photoelectron spectroscopy, Raman spectroscopy, Fourier transform infrared spectroscopy and nanoindentation. The N concentration showed a maximum of 35 at% at 20 A and decreased gradually with the arc currents. The films below 40 A consisted of linear polymeric-like component and sp2 graphitic cluster. With the increasing of the arc current from 20 to 40 A, the ID/IG rose and the photoluminescence (PL) fell gradually, which resulted from the development of the sp2 graphitic phase and the decrease of the polymeric-like phase. As a result, the CC bonds increased and sp3CN and sp2CN decreased. Above 40 A, with the increasing of arc currents, ID/IG fell and the PL increased gradually, which reflected the decreasing of sp2 graphitic phase and the modification of C and N atoms in sp2 cluster. The CC bonds and sp3CN fell and the sp2CN rose. The nanohardness of films showed increasing tendency with the arc currents. The variation of the relative ratio and the average energy of N-containing species and C-containing species at the atmosphere would be responsible for the change in the properties of films.

  17. Blast Furnace Granulated Coal Injection

    SciTech Connect

    1998-09-30

    Production levels on each furnace exceeded 7000 NTHM/day during July. The combined production of 14,326 was a result of lower coke rates and below average delay rates on both furnaces, The combined production was at its highest level since September 1997. In August, the combined productivity declined to less than 13,500 NTHM/day. Although D furnace maintained a production rate in excess of 7000 NTHM/day, C furnace was lower because of a castfloor breakout and subsequent five day repair from August 26-30. Despite the lower productivity in August, injected coal and furnace coke rates were very good during the month. During September, the operation was difficult as a result of higher delays on both furnaces. The combined average monthly delay rate was considerably above the twenty-month average of 113 minutes per day and the combined average monthly production was less than 14,000 NTHM/day. Higher furnace coke rates at lower coal injection levels also contributed to the decrease. Additionally, the coke rate on both furnaces was increased substantially and the injected coal rate was decreased in preparation for the high volatile Colorado coal trial that started on September 28. The furnace process results for this quarter are shown in Tables 1A and 1B. In addition, the last twelve months of injected coal and coke rates for each furnace are shown in Figures 1 and 2.

  18. Graphite Technology Development Plan

    SciTech Connect

    W. Windes; T. Burchell; M.Carroll

    2010-10-01

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

  19. High efficiency furnace

    SciTech Connect

    Hwang, K. S.; Koestler, D. J.

    1985-12-31

    Disclosed is a dwelling furnace having at least one clam-shell type primary heat exchanger in parallel orientation with a secondary heat exchanger, both the primary and secondary heat exchangers being vertically oriented relative to a furnace housing and parallel to the flow of air to be heated. The primary heat exchanger has a combustion chamber in the lower end thereof, and the lower end of the secondary heat exchanger exhausts into a tertiary heat exchanger oriented approximately perpendicular to the primary and secondary heat exchangers and horizontally relative to the housing, below the combustion chambers of the primary heat exchangers and below the exhaust outlet of the secondary heat exchanger. The tertiary heat exchanger includes a plurality of condensation tubes for retrieving the latent heat of condensation of the combustion gases. The furnace further comprises an induced draft blower for drawing combustion gases through the heat exchangers and inducting sufficient air to the combustion chamber of the primary heat exchanger for efficient combustion.

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

    NASA Astrophysics Data System (ADS)

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

    2014-01-01

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

  1. Carbon-free induction furnace

    DOEpatents

    Holcombe, Cressie E.; Masters, David R.; Pfeiler, William A.

    1985-01-01

    An induction furnace for melting and casting highly pure metals and alloys such as uranium and uranium alloys in such a manner as to minimize contamination of the melt by carbon derived from the materials and the environment within the furnace. The subject furnace is constructed of carbon free materials and is housed within a conventional vacuum chamber. The furnace comprises a ceramic oxide crucible for holding the charge of metal or alloy. The heating of the crucible is achieved by a plasma-sprayed tungsten susceptor surrounding the crucible which, in turn, is heated by an RF induction coil separated from the susceptor by a cylinder of inorganic insulation. The furnace of the present invention is capable of being rapidly cycled from ambient temperatures to about 1650.degree. C. for effectively melting uranium and uranium alloys without the attendant carbon contamination problems previously encountered when using carbon-bearing furnace materials.

  2. Non-carbon induction furnace

    DOEpatents

    Holcombe, C.E.; Masters, D.R.; Pfeiler, W.A.

    1984-01-06

    The present invention is directed to an induction furnace for melting and casting highly pure metals and alloys such as uranium and uranium alloys in such a manner as to minimize contamination of the melt by carbon derived from the materials and the environment within the furnace. The subject furnace is constructed of non-carbon materials and is housed within a conventional vacuum chamber. The furnace comprises a ceramic oxide crucible for holding the charge of metal or alloys. The heating of the crucible is achieved by a plasma-sprayed tungsten susceptor surrounding the crucible which, in turn, is heated by an rf induction coil separated from the susceptor by a cylinder of inorganic insulation. The furnace of the present invention is capable of being rapidly cycled from ambient temperatures to about 1650/sup 0/C for effectively melting uranium and uranium alloys without the attendant carbon contamination problems previously encountered when using carbon-bearing furnace materials.

  3. Modeling of thermal plasma arc technology FY 1994 report

    SciTech Connect

    Hawkes, G.L.; Nguyen, H.D.; Paik, S.; McKellar, M.G.

    1995-03-01

    The thermal plasma arc process is under consideration to thermally treat hazardous and radioactive waste. A computer model for the thermal plasma arc technology was designed as a tool to aid in the development and use of the plasma arc-Joule beating process. The value of this computer model is to: (a) aid in understanding the plasma arc-Joule beating process as applied to buried waste or exhumed buried waste, (b) help design melter geometry and electrode configuration, (c) calculate the process capability of vitrifying waste (i.e., tons/hour), (d) develop efficient plasma and melter operating conditions to optimize the process and/or reduce safety hazards, (e) calculate chemical reactions during treatment of waste to track chemical composition of off-gas products, and composition of final vitrified waste form and (f) help compare the designs of different plasma-arc facilities. A steady-state model of a two-dimensional axisymmetric transferred plasma arc has been developed and validated. A parametric analysis was performed that studied the effects of arc length, plasma gas composition, and input power on the temperatures and velocity profiles of the slag and plasma gas. A two-dimensional transient thermo-fluid model of the US Bureau of Mines plasma arc melter has been developed. This model includes the growth of a slag pool. The thermo-fluid model is used to predict the temperature and pressure fields within a plasma arc furnace. An analysis was performed to determine the effects of a molten metal pool on the temperature, velocity, and voltage fields within the slag. A robust and accurate model for the chemical equilibrium calculations has been selected to determine chemical composition of final waste form and off-gas based on the temperatures and pressures within the plasma-arc furnace. A chemical database has been selected. The database is based on the materials to be processed in the plasma arc furnaces.

  4. Metal vapor plasma behavior during vacuum arc remelting of alloy 718

    SciTech Connect

    Zanner, F.J.; Maguire, M.C.; Williamson, R.L. ); Adasczik, C.B. ); Roberts, R.R. ); Strohecker, R. )

    1992-01-01

    A production vacuum arc remelt (VAR) furnace was modified to enable direct viewing of the metal vapor arc and molten electrode tip during melting of 432 mm dia. alloy 718 electrodes into 508 mm dia. ingots. Diffuse and constricted arcing conditions were characterized using high speed cinematography, standard video format, and monochromatic imaging. Constricted arcing was observed while melting electrodes contaminated with oxide slag of the type used for refractory linings in vacuum induction furnaces. Monochromatic imaging was used in visualize the ion distribution in the arc plasma; these images clearly showed whether the arc operated in a diffuse or constricted model. Diffuse arc melting conditions were very similar to those previously reported in the literature for smaller laboratory sized melts.

  5. Metal vapor plasma behavior during vacuum arc remelting of alloy 718

    SciTech Connect

    Zanner, F.J.; Maguire, M.C.; Williamson, R.L.; Adasczik, C.B.; Roberts, R.R.; Strohecker, R.

    1992-05-01

    A production vacuum arc remelt (VAR) furnace was modified to enable direct viewing of the metal vapor arc and molten electrode tip during melting of 432 mm dia. alloy 718 electrodes into 508 mm dia. ingots. Diffuse and constricted arcing conditions were characterized using high speed cinematography, standard video format, and monochromatic imaging. Constricted arcing was observed while melting electrodes contaminated with oxide slag of the type used for refractory linings in vacuum induction furnaces. Monochromatic imaging was used in visualize the ion distribution in the arc plasma; these images clearly showed whether the arc operated in a diffuse or constricted model. Diffuse arc melting conditions were very similar to those previously reported in the literature for smaller laboratory sized melts.

  6. HIGH TEMPERATURE MICROSCOPE AND FURNACE

    DOEpatents

    Olson, D.M.

    1961-01-31

    A high-temperature microscope is offered. It has a reflecting optic situated above a molten specimen in a furnace and reflecting the image of the same downward through an inert optic member in the floor of the furnace, a plurality of spaced reflecting plane mirrors defining a reflecting path around the furnace, a standard microscope supported in the path of and forming the end terminus of the light path.

  7. Complex structure of the carbon arc discharge for synthesis of nanotubes

    NASA Astrophysics Data System (ADS)

    Vekselman, V.; Feurer, M.; Huang, T.; Stratton, B.; Raitses, Y.

    2017-06-01

    Comprehensive non-invasive spectroscopic techniques and electrical measurements of the carbon arc revealed two distinguishable plasma synthesis regions in the radial direction normal to the arc axis. These regions, which are defined as the arc core and the arc periphery, are shown to have very different compositions of carbon species with different densities and temperatures. The colder arc periphery is dominated by carbon diatomic molecules (C2), which are in the minority in the composition of the hot arc core. These differences are due to a highly non-uniform distribution of the arc current, which is mainly conducted through the arc core populated with carbon atoms and ions. Therefore, the ablation of the graphite anode is governed by the arc core, while the formation of carbon molecules occurs in the colder arc periphery. This result is consistent with previous predictions that the plasma environment in the arc periphery is suitable for synthesis of carbon nanotubes.

  8. Hot forging of graphite-carbide composites. Final report

    SciTech Connect

    Jenkins, G.M.; Holland, L.R.

    1998-07-15

    This project was aimed at hot shaping of titanium carbide/graphite and vanadium carbide/graphite composite materials by heating them to above 2000 degrees celsius and pressing into an electrographite die. The sample was to be a preformed cylinder of powdered graphite mixed with powdered titanium or vanadium, lightly sintered. The preform would be heated in a hot press and the titanium or vanadium would react with some of the graphite to form titanium or vanadium carbide. The remaining (excess) graphite would form a composite with the carbide, and this could then be deformed plastically at temperatures well below the onset of plasticity in pure graphite. There were to be two major thrusts in the research: In the first, an electron beam furnace at Sandia Laboratory was to be used for rapid heating of the sample, which would then be transferred into the press. The second thrust was to be entirely at Alabama A and M University, and here they intended to use a heated, controlled atmosphere press to forge the graphite/carbide preforms at a steady temperature and measure their viscosity as a function of temperature. This report discusses the progress made on this project.

  9. Elements of arc welding

    SciTech Connect

    Not Available

    1993-07-01

    This paper looks at the following arc welding techniques: (1) shielded metal-arc welding; (2) submerged-arc welding; (3) gas metal-arc welding; (4) flux-cored arc welding; (5) electrogas welding; (6) gas tungsten-arc welding; and (7) plasma-arc welding.

  10. Magnetically Damped Furnace (MDF)

    NASA Technical Reports Server (NTRS)

    1998-01-01

    The Magnetically Damped Furnace (MDF) breadboard is being developed in response to NASA's mission and goals to advance the scientific knowledge of microgravity research, materials science, and related technologies. The objective of the MDF is to dampen the fluid flows due to density gradients and surface tension gradients in conductive melts by introducing a magnetic field during the sample processing. The MDF breadboard will serve as a proof of concept that the MDF performance requirements can be attained within the International Space Station resource constraints.

  11. Water gas furnace

    SciTech Connect

    Gallaro, C.

    1985-12-03

    A water gas furnace comprising an outer container to provide a housing in which coke is placed into its lower part. A water container is placed within the housing. The coke is ignited and heats the water in the container converting it into steam. The steam is ejected into the coke, which together with air, produces water gas. Preferably, pumice stones are placed above the coke. The water gas is accepted into the pores of the pumice stones, where the heated pumice stones ignite the water gas, producing heat. The heat is extracted by a heat exchanger provided about the housing.

  12. Exothermic furnace module

    NASA Technical Reports Server (NTRS)

    Poorman, R. M. (Inventor)

    1982-01-01

    An exothermic furnace module is disclosed for processing materials in space which includes an insulated casing and a sample support, carried within the casing which supports a sample container. An exothermic heat source includes a plurality of segments of exothermic material stacked one upon another to produce a desired temperature profile when ignited. The exothermic material segments are constructed in the form of an annular element having a recess opening which defines an open central core throughout the vertical axis of the stacked exothermic material. The sample container is arranged within the core of the stacked exothermic heating material.

  13. Magnetically Damped Furnace (MDF)

    NASA Technical Reports Server (NTRS)

    1998-01-01

    The Magnetically Damped Furnace (MDF) breadboard is being developed in response to NASA's mission and goals to advance the scientific knowledge of microgravity research, materials science, and related technologies. The objective of the MDF is to dampen the fluid flows due to density gradients and surface tension gradients in conductive melts by introducing a magnetic field during the sample processing. The MDF breadboard will serve as a proof of concept that the MDF performance requirements can be attained within the International Space Station resource constraints.

  14. Experimental Observations and Numerical Prediction of Induction Heating in a Graphite Test Article

    SciTech Connect

    Jankowski, Todd A; Johnson, Debra P; Jurney, James D; Freer, Jerry E; Dougherty, Lisa M; Stout, Stephen A

    2009-01-01

    The induction heating coils used in the plutonium casting furnaces at the Los Alamos National Laboratory are studied here. A cylindrical graphite test article has been built, instrumented with thermocouples, and heated in the induction coil that is normally used to preheat the molds during casting operations. Preliminary results of experiments aimed at understanding the induction heating process in the mold portion of the furnaces are reported. The experiments have been modeled in COMSOL Multiphysics and the numerical and experimental results are compared to one another. These comparisons provide insight into the heating process and provide a benchmark for COMSOL calculations of induction heating in the mold portion of the plutonium casting furnaces.

  15. Cupola Furnace Computer Process Model

    SciTech Connect

    Seymour Katz

    2004-12-31

    The cupola furnace generates more than 50% of the liquid iron used to produce the 9+ million tons of castings annually. The cupola converts iron and steel into cast iron. The main advantages of the cupola furnace are lower energy costs than those of competing furnaces (electric) and the ability to melt less expensive metallic scrap than the competing furnaces. However the chemical and physical processes that take place in the cupola furnace are highly complex making it difficult to operate the furnace in optimal fashion. The results are low energy efficiency and poor recovery of important and expensive alloy elements due to oxidation. Between 1990 and 2004 under the auspices of the Department of Energy, the American Foundry Society and General Motors Corp. a computer simulation of the cupola furnace was developed that accurately describes the complex behavior of the furnace. When provided with the furnace input conditions the model provides accurate values of the output conditions in a matter of seconds. It also provides key diagnostics. Using clues from the diagnostics a trained specialist can infer changes in the operation that will move the system toward higher efficiency. Repeating the process in an iterative fashion leads to near optimum operating conditions with just a few iterations. More advanced uses of the program have been examined. The program is currently being combined with an ''Expert System'' to permit optimization in real time. The program has been combined with ''neural network'' programs to affect very easy scanning of a wide range of furnace operation. Rudimentary efforts were successfully made to operate the furnace using a computer. References to these more advanced systems will be found in the ''Cupola Handbook''. Chapter 27, American Foundry Society, Des Plaines, IL (1999).

  16. Two chamber reaction furnace

    DOEpatents

    Blaugher, R.D.

    1998-05-05

    A vertical two chamber reaction furnace is described. The furnace comprises a lower chamber having an independently operable first heating means for heating the lower chamber and a gas inlet means for admitting a gas to create an ambient atmosphere, and an upper chamber disposed above the lower chamber and having an independently operable second heating means for heating the upper chamber. Disposed between the lower chamber and the upper chamber is a vapor permeable diffusion partition. The upper chamber has a conveyor means for conveying a reactant there through. Of particular importance is the thallinating of long-length thallium-barium-calcium-copper oxide (TBCCO) or barium-calcium-copper oxide (BCCO) precursor tapes or wires conveyed through the upper chamber to thereby effectuate the deposition of vaporized thallium (being so vaporized as the first reactant in the lower chamber at a temperature between about 700 C and 800 C) on TBCCO or BCCO tape or wire (the second reactant) at its simultaneous annealing temperature in the upper chamber of about 800 to 950 C to thereby replace thallium oxide lost from TBCCO tape or wire because of the high annealing temperature or to deposit thallium on BCCO tape or wire. Continuously moving the tape or wire provides a single-step process that effectuates production of long-length TBCCO superconducting product. 2 figs.

  17. Two chamber reaction furnace

    DOEpatents

    Blaugher, Richard D.

    1998-05-05

    A vertical two chamber reaction furnace. The furnace comprises a lower chamber having an independently operable first heating means for heating the lower chamber and a gas inlet means for admitting a gas to create an ambient atmosphere, and an upper chamber disposed above the lower chamber and having an independently operable second heating means for heating the upper chamber. Disposed between the lower chamber and the upper chamber is a vapor permeable diffusion partition. The upper chamber has a conveyor means for conveying a reactant there through. Of particular importance is the thallinating of long-length thallium-barium-calcium-copper oxide (TBCCO) or barium-calcium-copper oxide (BCCO) precursor tapes or wires conveyed through the upper chamber to thereby effectuate the deposition of vaporized thallium (being so vaporized as the first reactant in the lower chamber at a temperature between about 700.degree. and 800.degree. C.) on TBCCO or BCCO tape or wire (the second reactant) at its simultaneous annealing temperature in the upper chamber of about 800.degree. to 950.degree. C. to thereby replace thallium oxide lost from TBCCO tape or wire because of the high annealing temperature or to deposit thallium on BCCO tape or wire. Continuously moving the tape or wire provides a single-step process that effectuates production of long-length TBCCO superconducting product.

  18. Fuel stoker and furnace

    SciTech Connect

    Schafer, T.L.; Schafer, G.L.; Swett, H.D.

    1984-02-14

    A furnace having a primary heat exchange unit also providing a combustion chamber, a secondary heat exchange unit connected by an upper crossover conduit to the primary heat exchange unit, and a tertiary heat exchange unit connected by a lower V-shaped crossover conduit to the secondary heat exchange unit. A third crossover conduit connects the V-shaped crossover conduit with the primary heat exchange unit. Vibrating means are provided between the secondary and tertiary heat exchange units to vibrate the walls thereof and dislodge clinging fly ash so that it falls into the V-shaped crossover conduit for removal by the screw conveyor. A burner assembly of a furnace includes a combustion air housing carrying a circular, stationary grate with an annular valley for carrying fuel during combustion. A central opening is connected to a fuel conveyor for introduction of fuel to the grate through the lower portion of the housing. Combustion air introduction conduits on the housing are remote from the fuel introduction passages and introduce air under pressure at the lower portion of the grate. An agitator and discharge ring is provided on the grate and is rotated on the grate by a suitable drive sprocket mechanism to agitate the fuel for more complete burning thereof and to remove burned ash. A horizontal burner plate is supported by a plurality of legs connected to the agitator and discharge ring over the grate to promote more complete combustion of the fuel.

  19. Blast furnace injection symposium: Proceedings

    SciTech Connect

    1996-12-31

    These proceedings contain 14 papers related to blast furnace injection issues. Topics include coal quality, coal grinding, natural gas injection, stable operation of the blast furnace, oxygen enrichment, coal conveying, and performance at several steel companies. All papers have been processed separately for inclusion on the data base.

  20. Heating rates in furnace atomic absorption using the L'vov platform

    USGS Publications Warehouse

    Koirtyohann, S.R.; Giddings, R.C.; Taylor, H.E.

    1984-01-01

    Heating rate profiles for the furnace tube wall, the furnace atmosphere, and a L'vov platform were established for a range of conditions in a cyclically heated graphite atomizer. The tube wall profile was made by direct observation with a recording optical pyrometer. The sodium line reversal method was used to establish the heating rate of the furnace atmosphere, and appearance temperatures for a series metals of differing volatility was used to establish platform profiles. The tube wall heating rate was nearly linear at 2240??C s- until the desired temperature was reached after which the temperature remained constant. The furnace atmosphere reached a given temperature 0.2-0.4 s later than the tube wall through most of the atomize cycle. The platform lagged the tube wall 0.5-0.8 s. Under typical operating conditions the furnace atmosphere was 100-200??C cooler than the tube wall and at nearly constant temperature when the analyte vaporized from the platform. The L'vov platform causes the cyclically heated commercial furnace to approximate the behavior of a constant temperature furnace during atomization. ?? 1984.