Linearization of calibration curves by aerosol carrier effect of CCl 4 vapor in electrothermal vaporization inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Kántor, Tibor; de Loos-Vollebregt, Margaretha T. C.

2005-03-01

Carbon tetrachloride vapor as gaseous phase modifier in a graphite furnace electrothermal vaporizer (GFETV) converts heavy volatile analyte forms to volatile and medium volatile chlorides and produces aerosol carrier effect, the latter being a less generally recognized benefit. However, the possible increase of polyatomic interferences in inductively coupled plasma mass spectrometry (GFETV-ICP-MS) by chlorine and carbon containing species due to CCl 4 vapor introduction has been discouraging with the use of low resolution, quadrupole type MS equipment. Being aware of this possible handicap, it was aimed at to investigate the feasibility of the use of this halogenating agent in ICP-MS with regard of possible hazards to the instrument, and also to explore the advantages under these specific conditions. With sample gas flow (inner gas flow) rate not higher than 900 ml min -1 Ar in the torch and 3 ml min -1 CCl 4 vapor flow rate in the furnace, the long-term stability of the instrument was ensured and the following benefits by the halocarbon were observed. The non-linearity error (defined in the text) of the calibration curves (signal versus mass functions) with matrix-free solution standards was 30-70% without, and 1-5% with CCl 4 vapor introduction, respectively, at 1 ng mass of Cu, Fe, Mn and Pb analytes. The sensitivity for these elements increased by 2-4-fold with chlorination, while the relative standard deviation (RSD) was essentially the same (2-5%) for the two cases in comparison. A vaporization temperature of 2650 °C was required for Cr in Ar atmosphere, while 2200 °C was sufficient in Ar + CCl 4 atmosphere to attain complete vaporization. Improvements in linear response and sensitivity were the highest for this least volatile element. The pyrolytic graphite layer inside the graphite tube was protected by the halocarbon, and tube life time was further increased by using traces of hydrocarbon vapor in the external sheath gas of the graphite furnace. Details of the modification of the gas supply for HGA-600MS furnace and the design of the volatilization device are described.

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.

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.

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.

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...

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.

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. Copyright © 2013 Elsevier B.V. All rights reserved.

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…

75 FR 76026 - United States v. Graftech International Ltd., Et al.; Proposed Final Judgment and Competitive...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-12-07

... and other inputs to form cylinders that are shot through with electricity and baked to produce... electricity into the furnace, heating the furnace and melting scrap steel. 11. Graphite electrodes oxidize and... consumption of graphite electrodes. 12. Petroleum needle coke, relative to other varieties of coke, is...

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.

Graphite fiber/copper composites prepared by spontaneous infiltration

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Schnellverfahren zur flammenlosen AAS-Bestimmung von Spurenelementen in geologischen Proben

NASA Astrophysics Data System (ADS)

Schrön, W.; Bombach, G.; Beuge, P.

This paper reports experience with direct quantitative trace element determinations in powdered geological samples by nameless atomic absorption spectroscopy. Two methods were explored. The first one is based on the production of a sample aerosol by laser radiation in a specifically designed sample chamber and the subsequent transport of the aerosol into a graphite tube, which has been preheated to a stable temperature. This technique is suited for a large range of concentration and is relatively free from matrix interferences. The technique was tested for the elements Ag, As, Bi, Cd, Co, Mn, Ni, Pb, Sb, Se, Sr and Tl. The described sample chamber can be also used in combination with other spcctroscopic techniques. The second method explored permits the quantitative determination of trace elements at very low concentrations. Essentially an accurately weighed amount of sample is placed on a graphite rod and introduced into a graphite furnace by inserting the rod through the sample injection port. Atomization takes place also under stable temperature conditions. Using this technique detection limits were found to be 10 -11 g for Ag, 2 × 10 -11 g for Cd and 10 -10 g for Sb in silicate materials.

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

NASA Astrophysics Data System (ADS)

Kowalewska, Zofia

2011-07-01

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

Time series prediction in the case of nonlinear loads by using ADALINE and NAR neural networks

NASA Astrophysics Data System (ADS)

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

2018-01-01

This paper presents a study regarding the time series prediction in the case of an electric arc furnace. The considered furnace is a three phase load and it is used to melt scrap in order to obtain liquid steel. The furnace is powered by a three-phase electrical supply and therefore has three graphite electrodes. The furnace is a nonlinear load that can influence the equipment connected to the same electrical power supply network. The nonlinearity is given by the electric arc that appears at the furnace between the graphite electrode and the scrap. Because of the disturbances caused by the electric arc furnace during the elaboration process of steel it is very useful to predict the current of the electric arc and the voltage from the measuring point in the secondary side of the furnace transformer. In order to make the predictions were used ADALINE and NAR neural networks. To train the networks and to make the predictions were used data acquired from the real technological plant.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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)more » 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.« less

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

EPA Science Inventory

The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

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.

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).

Vaporization and atomization of uranium in a graphite tube electrothermal vaporizer: a mechanistic study using electrothermal vaporization inductively coupled plasma mass spectrometry and graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Goltz, D. M.; Grégoire, D. C.; Byrne, J. P.; Chakrabarti, C. L.

1995-07-01

The mechanism of vaporization and atomization of U in a graphite tube electrothermal vaporizer was studied using graphite furnace atomic absorption spectrometry (GFAAS) and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). Graphite furnace AAS studies indicate U atoms are formed at temperatures above 2400°C. Using ETV-ICP-MS, an appearance temperature of 1100°C was obtained indicating that some U vaporizes as U oxide. Although U carbides form at temperatures above 2000°C, ETV-ICP-MS studies show that they do not vaporize until 2600°C. In the temperature range between 2200°C and 2600°C, U atoms in GFAAS are likely formed by thermal dissociation of U oxide, whereas at higher temperatures, U atoms are formed via thermal dissociation of U carbide. The origin of U signal suppression in ETV-ICP-MS by NaCl was also investigated. At temperatures above 2000°C, signal suppression may be caused by the accelerated rate of formation of carbide species while at temperatures below 2000°C, the presence of NaCl may cause intercalation of the U in the graphite layers resulting in partial retention of U during the vaporization step. The use of 0.3% freon-23 (CHF 3) mixed with the argon carrier gas was effective in preventing the intercalation of U in graphite and U carbide formation at 2700°C.

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.

BUNDLE: A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

NASA Technical Reports Server (NTRS)

Carrasquillo, Edgar J.; Griffin, Mark R.; Hammond, Monica S.; Johnson, Martin L.; Grugel, R. N.

2000-01-01

NASA Marshall Space Flight Center has developed a novel directional solidification furnace prototype for processing metals and alloys experiments in a microgravity environment. The BUNDLE (Bridgman Unidirectional Dendrite in Liquid Experiment) furnace is intended to accommodate the science requirements of Flight Definition Principle Investigators studying cellular/dendritic growth in aluminum and lead alloys at processing temperatures up to 1200 C. The furnace implements a number of innovative features to achieve high thermal gradients and quench rates in a low-power, light-weight design. These include a pyrolytic boron nitride/graphite composite heating element surrounded by layers of self-supporting refractory metal shielding, and a graphite fiber enhanced cold zone allowing high levels of heat extraction from the sample crucible. Novel to the BUNDLE design is an in-situ helium gas quench capability that ensures rapid freezing of the solidifying region (mushy zone) of the metal sample within the furnace without sample disturbance prior to quenching; this is a stringent requirement for subsequent analysis and understanding of microstructural development. The experiment hardware concept features multiple furnaces that may be "bundled" together so many samples, currently up to eight, can be processed at one time. The design of BUNDLE is flexible enough to be implemented on the Shuttle and Space Station in a number of locations (SpaceHab, Express Rack, MPESS, ISPR, etc). BUNDLE prototype furnaces have directionally solidified and quenched 1cm diameter lead - 5.8 weight percent antimony and aluminum - 4 weight percent copper alloys. Quenching of the mushy zone, as recorded by in-situ thermocouples, occurred on the order of 0.5 seconds or less, a rate within the PI's requirements. Subsequent metallographic examination revealed the solidified microstructure to be, as expected, unidirectional. Both the dendrite tips and the eutectic reaction were planar in nature indicating uniform axial heat flow. Delineation between the growing dendrites and eutectic structure with the "quenched-in" liquid was sharp, attesting to the efficacy of the helium quench. BUNDLE's conception, development, capability, and adaptability are presented (in view of Flight PI's needs and science requirements) through viewgraphs depicting actual hardware, generated thermal analysis, and micrographs prepared from BUNDLE processed, flight-like samples.

BUNDLE - A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

NASA Technical Reports Server (NTRS)

Carrasquillo, Edgar J.; Griffin, Mark R.; Hammond, Monica S.; Johnson, Martin L.; Grugel, R. N.

2001-01-01

NASA Marshall Space Flight Center has developed a novel directional solidification furnace prototype for processing metals and alloys experiments in a microgravity environment. The BUNDLE (Bridgman Unidirectional Dendrite in Liquid Experiment) furnace is intended to accommodate the science requirements of Flight Definition Principle Investigators studying cellular/dendritic growth in aluminum and lead alloys at processing temperatures up to 1200 C. The furnace implements a number of innovative features to achieve high thermal gradients and quench rates in a low-power, light-weight design. These include a pyrolytic boron nitride/graphite composite heating element surrounded by layers of self-supporting refractory metal shielding, and a graphite fiber enhanced cold zone allowing high levels of heat extraction from the sample crucible. Novel to the BUNDLE design is an in-situ helium gas quench capability that ensures rapid freezing of the solidifying region (mushy zone) of the metal sample within the furnace without sample disturbance prior to quenching; this is a stringent requirement for subsequent analysis and understanding of microstructural development. The experiment hardware concept features multiple furnaces that may be "bundled" together so many samples, currently up to eight, can be processed at one time. The design of BUNDLE is flexible enough to be implemented on the Shuttle and Space Station in a number of locations (SpaceHab, Express Rack, MPESS, ISPR, etc). BUNDLE prototype furnaces have directionally solidified and quenched 1cm diameter lead - 5.8 weight percent antimony and aluminum - 4 weight percent copper alloys. Quenching of the mushy zone, as recorded by in-situ thermocouples, occurred on the order of 0.5 seconds or less, a rate within the PI's requirements. Subsequent metallographic examination revealed the solidified microstructure to be, as expected, unidirectional. Both the dendrite tips and the eutectic reaction were planar in nature indicating uniform axial heat flow. Delineation between the growing dendrites and eutectic structure with the "quenched-in" liquid was sharp, attesting to the efficacy of the helium quench. BUNDLE's conception, development, capability, and adaptability are presented (in view of Flight PI's needs and science requirements) through viewgraphs depicting actual hardware, generated thermal analysis, and micrographs prepared from BUNDLE processed, flight-like samples.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL WIPE SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

EPA Science Inventory

The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

A phase-field approach to model multi-axial and microstructure dependent fracture in nuclear grade graphite

DOE PAGES

Chakraborty, Pritam; Sabharwall, Piyush; Carroll, Mark C.

2016-04-07

The fracture behavior of nuclear grade graphites is strongly influenced by underlying microstructural features such as the character of filler particles, and the distribution of pores and voids. These microstructural features influence the crack nucleation and propagation behavior, resulting in quasi-brittle fracture with a tortuous crack path and significant scatter in measured bulk strength. This paper uses a phase-field method to model the microstructural and multi-axial fracture in H-451, a historic variant of nuclear graphite that provides the basis for an idealized study on a legacy grade. The representative volume elements are constructed from randomly located pores with random sizemore » obtained from experimentally determined log-normal distribution. The representative volume elements are then subjected to simulated multi-axial loading, and a reasonable agreement of the resulting fracture stress with experiments is obtained. Finally, quasi-brittle stress-strain evolution with a tortuous crack path is also observed from the simulations and is consistent with experimental results.« less

Evaluation of methods for trace-element determination with emphasis on their usability in the clinical routine laboratory.

PubMed

Bolann, B J; Rahil-Khazen, R; Henriksen, H; Isrenn, R; Ulvik, R J

2007-01-01

Commonly used techniques for trace-element analysis in human biological material are flame atomic absorption spectrometry (FAAS), graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). Elements that form volatile hydrides, first of all mercury, are analysed by hydride generation techniques. In the absorption techniques the samples are vaporized into free, neutral atoms and illuminated by a light source that emits the atomic spectrum of the element under analysis. The absorbance gives a quantitative measure of the concentration of the element. ICP-AES and ICP-MS are multi-element techniques. In ICP-AES the atoms of the sample are excited by, for example, argon plasma at very high temperatures. The emitted light is directed to a detector, and the optical signals are processed to values for the concentrations of the elements. In ICP-MS a mass spectrometer separates and detects ions produced by the ICP, according to their mass-to-charge ratio. Dilution of biological fluids is commonly needed to reduce the effect of the matrix. Digestion using acids and microwave energy in closed vessels at elevated pressure is often used. Matrix and spectral interferences may cause problems. Precautions should be taken against trace-element contamination during collection, storage and processing of samples. For clinical problems requiring the analysis of only one or a few elements, the use of FAAS may be sufficient, unless the higher sensitivity of GFAAS is required. For screening of multiple elements, however, the ICP techniques are preferable.

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.

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.

Role of iron modifier on boron atomization process using graphite furnace-atomic absorption spectrometry based on speciation of iron using X-ray absorption fine structure

NASA Astrophysics Data System (ADS)

Yamamoto, Yuhei; Tagami, Azusa; Shiarasaki, Toshihiro; Yonetani, Akira; Yamamoto, Takashi; Imai, Shoji

2018-04-01

The role of an Fe modifier on boron atomization process using graphite furnace-atomic absorbance spectrometry was investigated using a spectroscopic approach. The initial state of the Fe modifier in a pyrolytic graphite (PG) furnace was trivalent. With an increase in pyrolysis temperature, the Fe modifier was reduced in a stepwise manner. Fe2O3 and Fe3O4 were dominant at pyrolysis temperatures below 1300 K. From 1300 to 1500 K, FeO was dominant. At temperatures higher than 1700 K, Fe metal was dominant. After a drying step, 17.7% of the initial B remained in the PG furnace. After the pyrolysis step at 773 K, the residual fraction of B was similar to that after the drying step. After the pyrolysis step at a temperature of 1073 K, the residual fraction was 11.7%. At pyrolysis temperatures > 1738 K, the residual fraction was <3.3% (

Pigment identification in artwork using graphite furnace atomic absorption spectrometry.

PubMed

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

2004-06-17

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

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.

Determination of selected elements in whole coal and in coal ash from the eight argonne premium coal samples by atomic absorption spectrometry, atomic emission spectrometry, and ion-selective electrode

USGS Publications Warehouse

Doughten, M.W.; Gillison, J.R.

1990-01-01

Methods for the determination of 24 elements in whole coal and coal ash by inductively coupled argon plasma-atomic emission spectrometry, flame, graphite furnace, and cold vapor atomic absorption spectrometry, and by ion-selective electrode are described. Coal ashes were analyzed in triplicate to determine the precision of the methods. Results of the analyses of NBS Standard Reference Materials 1633, 1633a, 1632a, and 1635 are reported. Accuracy of the methods is determined by comparison of the analysis of standard reference materials to their certified values as well as other values in the literature.

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. Copyright © 2016 Elsevier Ltd. All rights reserved.

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). Copyright © 2015 Elsevier B.V. All rights reserved.

Competitive adsorption of copper(II), cadmium(II), lead(II) and zinc(II) onto basic oxygen furnace slag.

PubMed

Xue, Yongjie; Hou, Haobo; Zhu, Shujing

2009-02-15

Polluted and contaminated water can often contain more than one heavy metal species. It is possible that the behavior of a particular metal species in a solution system will be affected by the presence of other metals. In this study, we have investigated the adsorption of Cd(II), Cu(II), Pb(II), and Zn(II) onto basic oxygen furnace slag (BOF slag) in single- and multi-element solution systems as a function of pH and concentration, in a background solution of 0.01M NaNO(3). In adsorption edge experiments, the pH was varied from 2.0 to 13.0 with total metal concentration 0.84mM in the single element system and 0.21mM each of Cd(II), Cu(II), Pb(II), and Zn(II) in the multi-element system. The value of pH(50) (the pH at which 50% adsorption occurs) was found to follow the sequence Zn>Cu>Pb>Cd in single-element systems, but Pb>Cu>Zn>Cd in the multi-element system. Adsorption isotherms at pH 6.0 in the multi-element systems showed that there is competition among various metals for adsorption sites on BOF slag. The adsorption and potentiometric titrations data for various slag-metal systems were modeled using an extended constant-capacitance surface complexation model that assumed an ion-exchange process below pH 6.5 and the formation of inner-sphere surface complexes at higher pH. Inner-sphere complexation was more dominant for the Cu(II), Pb(II) and Zn(II) systems.

Ultra-High Temperature ContinuousReactors based on Electro-thermal FluidizedBed Concept

DOE PAGES

Fedorov, Sergiy S.; Rohatgi, Upendra Singh; Barsukov, Igor V.; ...

2015-12-08

This paper presents the results of research and development in high-temperature (i.e. 2,000- 3,000ºС) continuous furnaces operating on the principle of electro-thermal fluidized bed for the purification of recycled, finely sized carbon materials. The basis of this fluidized bed furnace is specific electrical resistance and a new correlation has been developed to predict specific electrical resistance for the natural graphite-based precursors entering the fluidized bed reactor This correlation has been validated with the data from a fully functional pilot furnace whose throughput capacity is 10 kg per hour built as part of this work. Data collected in the course ofmore » graphite refining experiments demonstrated that difference between the calculated and measured values of specific electrical resistance of fluidized bed does not exceed 25%. It was concluded that due to chaotic nature of electro-thermal fluidized bed reactors this discrepancy is acceptable. The fluid mechanics of the three types of operating regimes, have been described. The numerical relationships obtained as part of this work allowed proposing an algorithm for selection of technological operational modes with large- scale high-temperature furnaces rated for throughputs of several tons of product per hour. Optimizations proposed now allow producing natural graphite-based end product with the purity level of 99.98+ wt%C which is the key passing criteria for applications in the advanced battery markets.« less

Characterization of Austempered Ferritic Ductile Iron

NASA Astrophysics Data System (ADS)

Dakre, Vinayak S.; Peshwe, D. R.; Pathak, S. U.; Likhite, A. A.

2018-04-01

The ductile iron (DI) has graphite nodules enclose in ferrite envelop in pearlitic matrix. The pearlitic matrix in DI was converted to ferritic matrix through heat treatment. This heat treatment includes austenitization of DI at 900°C for 1h, followed by furnace cooling to 750°C & hold for 1h, then again furnace cooling to 690°C hold for 2h, then samples were allowed to cool in furnace. The new heat treated DI has graphite nodules in ferritic matrix and called as ferritic ductile iron (FDI). Both DIs were austenitized at 900°C for 1h and then quenched into salt bath at 325°C. The samples were soaked in salt bath for 60, 120, 180, 240 and 300 min followed by air cooling. The austempered samples were characterized with help of optical microscopy, SEM and X-ray diffraction analysis. Austempering of ferritic ductile iron resulted in finer ausferrite matrix as compared to ADI. Area fraction of graphite, ferrite and austenite were determining using AXIOVISION-SE64 software. Area fraction of graphite was more in FDI than that of as cast DI. The area fraction of graphite remains unaffected due to austempering heat treatment. Ausferritic matrix coarsened (feathered) with increasing in austempering time for both DI and FDI. Bulk hardness test was carried on Rockwell Hardness Tester with load of 150 kgf and diamond indenter. Hardness obtained in as cast DI is 28 HRC which decreased to 6 HRC in FDI due conversion of pearlitic matrix to ferritic matrix. Hardness is improved by austempering process.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Sulfur determination in coal using molecular absorption in graphite filter vaporizer.

PubMed

Jim, Gibson; Katskov, Dmitri; Tittarelli, Paolo

2011-02-15

The vaporization of sulfur containing samples in graphite vaporizers for atomic absorption spectrometry is accompanied by modification of sulfur by carbon and, respectively, appearance at high temperature of structured molecular absorption in 200-210 nm wavelength range. It has been proposed to employ the spectrum for direct determination of sulfur in coal; soundness of the suggestion is evaluated by analysis of coal slurry using low resolution CCD spectrometer with continuum light source coupled to platform or filter furnace vaporizers. For coal in platform furnace losses of the analyte at low temperature and strong spectral background from the coal matrix hinder the determination. Both negative effects are significantly reduced in filter furnace, in which sample vapor efficiently interacts with carbon when transferred through the heated graphite filter. The method is verified by analysis of coals with sulfur content within 0.13-1.5% (m/m) range. The use of coal certified reference material for sulfur analyte addition to coal slurry permitted determination with random error 5-12%. Absolute and relative detection limits for sulfur in coal are 0.16 μg and 0.02 mass%, respectively. Copyright © 2010 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gregoire, D.C.; Goltz, D.M.; Chakrabarti, C.L.

Graphite furnace atomic absorption spectrometry (GFAAS) is an insensitive technique for determination of uranium. Experiments were conducted using electrothermal vaporization inductively coupled plasma mass spectrometry to investigate the atomization and vaporization of atomic and molecular uranium species in the graphite furnace. ETV-ICP-MS signals for uranium were observed at temperatures well below the appearance temperature of uranium atoms suggesting the vaporization of molecular uranium oxide at temperatures below 2000{degrees}C. Examination of individual uranium ETV-ICP-MS signals reveals the vaporization of uranium carbide at temperatures above 2600{degrees}C. Chemical modifiers such as 0.2% HF and 0.1% CHF{sub 3} in the argon carrier gas, weremore » ineffective in preventing the formation of uranium carbide at 2700{degrees}C. Vaporization of uranium from a tungsten surface using tungsten foil inserted into the graphite tube prevented the formation of uranium carbide and eliminated the ETV-ICP-MS signal suppression caused by a sodium chloride matrix.« less

Back-extraction of trace elements from organometallic-halide extracts for determination by flameless atomic absorption spectrometry

USGS Publications Warehouse

Clark, J.R.; Viets, J.G.

1981-01-01

The Methyl isobutyl ketone-Amine synerGistic Iodkte Complex (MAGIC) extraction system offers the advantage that a large number of trace elements can be rapidly determined with a single sample preparation procedure. However, many of the elements extracted by the MAGIC system form volatile organometallic halide salts when the organic extract is heated in the graphite furnace. High concentrations of some elements such as Cu and Zn extracted by the system from anomalous geological samples produce serious interferences when certain other elements are determined by flameless atomic absorption. Stripping systems have been developed using solutions of HNO3, H2SO4, and CH3COOH individually or combined with H2O2 in order to circumvent these problems. With these systems most of the elements in the organic extract can be sequentially stripped into an aqueous phase. Organometallic volatilization and the most serious interelement interferences, therefore, can be eliminated by stripping with various combinations of reagents in a series of steps.

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

[Determination of metal elements in Achyranthis bidentatae radix from various habitats].

PubMed

Tu, Wan-Qian; Zhang, Liu-Ji

2011-12-01

To establish an atomic absorption spectrometry method for determination of the contents of metal elements in Achyranthis Bidentatae Radix and analyze 21 batches of samples from different areas. Fe, Mn, Ca, Mg, K, Zn and Cu were detected by atomic absorption spectrometry with hydrogen flame detector, Pb, As and Cd were detected by graphite furnace atomic absorption, Hg was detected by cold atomic absorption. The heavy metal contents met the requirement of Chinese Pharmacopoeia. The contents of K, Mg, Cu and Mn in the samples of geo-authentic areas were higher,while the contents of Fe, Zn, Hg and Pb in the samples of non-authentic areas were higher. This method is sample, accurate, repeatable and could be used to evaluate the quality of Achyranthis Bidentatae Radix.

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

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.

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

PubMed

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

2018-03-01

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

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

NASA Astrophysics Data System (ADS)

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

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

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

PubMed

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

2014-01-01

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

Construction material processed using lunar simulant in various environments

NASA Technical Reports Server (NTRS)

Chase, Stan; Ocallaghan-Hay, Bridget; Housman, Ralph; Kindig, Michael; King, John; Montegrande, Kevin; Norris, Raymond; Vanscotter, Ryan; Willenborg, Jonathan; Staubs, Harry

1995-01-01

The manufacture of construction materials from locally available resources in space is an important first step in the establishment of lunar and planetary bases. The objective of the CoMPULSIVE (Construction Material Processed Using Lunar Simulant In Various Environments) experiment is to develop a procedure to produce construction materials by sintering or melting Johnson Space Center Simulant 1 (JSC-1) lunar soil simulant in both earth-based (1-g) and microgravity (approximately 0-g) environments. The characteristics of the resultant materials will be tested to determine its physical and mechanical properties. The physical characteristics include: crystalline, thermal, and electrical properties. The mechanical properties include: compressive tensile, and flexural strengths. The simulant, placed in a sealed graphite crucible, will be heated using a high temperature furnace. The crucible will then be cooled by radiative and forced convective means. The core furnace element consists of space qualified quartz-halogen incandescent lamps with focusing mirrors. Sample temperatures of up to 2200 C are attainable using this heating method.

Non-destructive control of graphite electrodes with use of current displacement effect

NASA Astrophysics Data System (ADS)

Myatezh, A. V.; Malozyomov, B. V.; Smirnov, M. A.

2017-10-01

The work is devoted to methods of nondestructive diagnostics and their use for solving the problem of diagnosing various defects in solid surface of graphite electrodes used in steelmaking furnaces. Various non-destructive control methods of materials are analyzed. In the article, methods of eddy-current defectoscopy of graphite electrodes are considered. Rationalization of the sensitivity increase of the method and localization of damage is described. Imitating modeling of electromagnetic processes was executed; results were made and conclusions were drawn.

Genetic algorithms for multicriteria shape optimization of induction furnace

NASA Astrophysics Data System (ADS)

Kůs, Pavel; Mach, František; Karban, Pavel; Doležel, Ivo

2012-09-01

In this contribution we deal with a multi-criteria shape optimization of an induction furnace. We want to find shape parameters of the furnace in such a way, that two different criteria are optimized. Since they cannot be optimized simultaneously, instead of one optimum we find set of partially optimal designs, so called Pareto front. We compare two different approaches to the optimization, one using nonlinear conjugate gradient method and second using variation of genetic algorithm. As can be seen from the numerical results, genetic algorithm seems to be the right choice for this problem. Solution of direct problem (coupled problem consisting of magnetic and heat field) is done using our own code Agros2D. It uses finite elements of higher order leading to fast and accurate solution of relatively complicated coupled problem. It also provides advanced scripting support, allowing us to prepare parametric model of the furnace and simply incorporate various types of optimization algorithms.

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).

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 . Copyright © 2017 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Numerical Study of the Reduction Process in an Oxygen Blast Furnace

NASA Astrophysics Data System (ADS)

Zhang, Zongliang; Meng, Jiale; Guo, Lei; Guo, Zhancheng

2016-02-01

Based on computational fluid dynamics, chemical reaction kinetics, principles of transfer in metallurgy, and other principles, a multi-fluid model for a traditional blast furnace was established. The furnace conditions were simulated with this multi-fluid mathematical model, and the model was verified with the comparison of calculation and measurement. Then a multi-fluid model for an oxygen blast furnace in the gasifier-full oxygen blast furnace process was established based on this traditional blast furnace model. With the established multi-fluid model for an oxygen blast furnace, the basic characteristics of iron ore reduction process in the oxygen blast furnace were summarized, including the changing process of the iron ore reduction degree and the compositions of the burden, etc. The study found that compared to the traditional blast furnace, the magnetite reserve zone in the furnace shaft under oxygen blast furnace condition was significantly reduced, which is conducive to the efficient operation of blast furnace. In order to optimize the oxygen blast furnace design and operating parameters, the iron ore reduction process in the oxygen blast furnace was researched under different shaft tuyere positions, different recycling gas temperatures, and different allocation ratios of recycling gas between the hearth tuyere and the shaft tuyere. The results indicate that these three factors all have a substantial impact on the ore reduction process in the oxygen blast furnace. Moderate shaft tuyere position, high recycling gas temperature, and high recycling gas allocation ratio between hearth and shaft could significantly promote the reduction of iron ore, reduce the scope of the magnetite reserve zone, and improve the performance of oxygen blast furnace. Based on the above findings, the recommendations for improvement of the oxygen blast furnace design and operation were proposed.

The Determination of Metals in Sediment Pore Waters and in 1N HCl-Extracted Sediments by ICP-MS

USGS Publications Warehouse

May, T.W.; Wiedmeyer, Ray H.; Brumbaugh, W.G.; Schmitt, C.J.

1997-01-01

Concentrations of metals in sediment interstitial water (pore water) and those extractable from sediment with weak acids can provide important information about the bioavailability and toxicological effects of such contaminants. The highly variable nature of metal concentrations in these matrices requires instrumentation with the detection limit capability of graphite furnace atomic absorption and the wide dynamic linear range capability of ICP-OES. These criteria are satisfied with ICP-MS instrumentation. We investigated the performance of ICP-MS in the determination of certain metals from these matrices. The results for three metals were compared to those determined by graphite furnace atomic absorption spectroscopy. It was concluded that ICP-MS was an excellent instrumental approach for the determination of metals in these matrices.

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.

Self-tuning multivariable pole placement control of a multizone crystal growth furnace

NASA Technical Reports Server (NTRS)

Batur, C.; Sharpless, R. B.; Duval, W. M. B.; Rosenthal, B. N.

1992-01-01

This paper presents the design and implementation of a multivariable self-tuning temperature controller for the control of lead bromide crystal growth. The crystal grows inside a multizone transparent furnace. There are eight interacting heating zones shaping the axial temperature distribution inside the furnace. A multi-input, multi-output furnace model is identified on-line by a recursive least squares estimation algorithm. A multivariable pole placement controller based on this model is derived and implemented. Comparison between single-input, single-output and multi-input, multi-output self-tuning controllers demonstrates that the zone-to-zone interactions can be minimized better by a multi-input, multi-output controller design. This directly affects the quality of crystal grown.

Design and Development of Tilting Rotary Furnace

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Heating rates in furnace atomic absorption using the L'vov platform

USGS Publications Warehouse

Koirtyohann, S.R.; Giddings, R.C.; Taylor, Howard 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.

Determination of lead in flour samples directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Tinas, Hande; Ozbek, Nil; Akman, Suleyman

2018-02-01

In this study, lead concentrations in various flour samples were determined by high-resolution continuum source graphite furnace atomic absorption spectrometry with solid sampling. Since samples were analyzed directly, the risks and disadvantages of sample digestion were eliminated. Solid flour samples were dried, weighed on the platforms, Pd was added as a modifier and introduced directly into a graphite tube using a manual solid sampler. Platforms and tubes were coated with Zr. The optimized pyrolysis and atomization temperatures were 800 °C and 2200 °C, respectively. The sensitivities of lead in various flour certified reference materials (CRMs) and aqueous standards were not significantly different. Therefore, aqueous standards were safely used for calibration. The absolute limit of detection and characteristic mass were 7.2 pg and 9.0 pg of lead, respectively. The lead concentrations in different types of flour samples were found in the range of 25-52 μg kg- 1. Finally, homogeneity factors representing the heterogeneity of analyte distribution for lead in flour samples were determined.

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

Evaluation of inorganic elements in cat's claw teas using ICP OES and GF AAS.

PubMed

Pereira, João B; Dantas, Kelly G F

2016-04-01

The determination of Ba, Ca, Cu, Fe, Mg, Mn, P, Pb, and Zn by inductively coupled plasma optical emission spectrometry (ICP OES), and Se by graphite furnace atomic absorption spectrometry (GF AAS), has been carried out in dry matter and teas from 11 samples of the cat's claw plant. The accuracy and precision values were verified against GBW 07604 (Poplar leaves) certified reference material and by the recovery test. Results showed a high content of Ca in the medicinal plant studied, followed by Mg and P. The values obtained showed that the elements studied have different concentrations depending on the method of tea preparation. The highest levels were observed in Ca and Mg, and the lowest for Se and Pb, by both infusion and decoction. Teas prepared from this plant were found to be at safe levels for human consumption, and may be suitable as sources of these elements in the human diet. Copyright © 2015 Elsevier Ltd. All rights reserved.

Microgravity

NASA Image and Video Library

2001-06-05

This scale model depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Here the transparent furnace is extracted for servicing. Key elements are labeled in other images (0101754, 0101829, 0101830, and TBD).

Improved Blackbody Temperature Sensors for a Vacuum Furnace

NASA Technical Reports Server (NTRS)

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

2009-01-01

Some improvements have been made in the design and fabrication of blackbody sensors (BBSs) used to measure the temperature of a heater core in a vacuum furnace. Each BBS consists of a ring of thermally conductive, high-melting-temperature material with two tantalum-sheathed thermocouples attached at diametrically opposite points. The name "blackbody sensor" reflects the basic principle of operation. Heat is transferred between the ring and the furnace heater core primarily by blackbody radiation, heat is conducted through the ring to the thermocouples, and the temperature of the ring (and, hence, the temperature of the heater core) is measured by use of the thermocouples. Two main requirements have guided the development of these BBSs: (1) The rings should have as high an emissivity as possible in order to maximize the heat-transfer rate and thereby maximize temperature-monitoring performance and (2) the thermocouples must be joined to the rings in such a way as to ensure long-term, reliable intimate thermal contact. The problem of fabricating a BBS to satisfy these requirements is complicated by an application-specific prohibition against overheating and thereby damaging nearby instrumentation leads through the use of conventional furnace brazing or any other technique that involves heating the entire BBS and its surroundings. The problem is further complicated by another application-specific prohibition against damaging the thin tantalum thermocouple sheaths through the use of conventional welding to join the thermocouples to the ring. The first BBS rings were made of graphite. The tantalum-sheathed thermocouples were attached to the graphite rings by use of high-temperature graphite cements. The ring/thermocouple bonds thus formed were found to be weak and unreliable, and so graphite rings and graphite cements were abandoned. Now, each BBS ring is made from one of two materials: either tantalum or a molybdenum/titanium/zirconium alloy. The tantalum-sheathed thermocouples are bonded to the ring by laser brazing. The primary advantage of laser brazing over furnace brazing is that in laser brazing, it is possible to form a brazed connection locally, without heating nearby parts to the flow temperature of the brazing material. Hence, it is possible to comply with the prohibition against overheating nearby instrumentation leads. Also, in laser brazing, unlike in furnace brazing, it is possible to exert control over the thermal energy to such a high degree that it becomes possible to braze the thermocouples to the ring without burning through the thin tantalum sheaths on the thermocouples. The brazing material used in the laser brazing process is a titanium-boron paste. This brazing material can withstand use at temperatures up to about 1,400 C. In thermal-cycling tests performed thus far, no debonding between the rings and thermocouples has been observed. Emissivity coatings about 0.001 in. (.0.025 mm) thick applied to the interior surfaces of the rings have been found to improve the performance of the BBS sensors by raising the apparent emissivities of the rings. In thermal-cycling tests, the coatings were found to adhere well to the rings.

Soft X-Ray Absorption Spectroscopy of High-Abrasion-Furnace Carbon Black

DOE Office of Scientific and Technical Information (OSTI.GOV)

Muramatsu, Yasuji; Harada, Ryusuke; Gullikson, Eric M.

2007-02-02

The soft x-ray absorption spectra of high-abrasion-furnace carbon black were measured to obtain local-structure/chemical-states information of the primary particles and/or crystallites. The soft x-ray absorption spectral features of carbon black represent broader {pi}* and {sigma}* peak structures compared to highly oriented pyrolytic graphite (HOPG). The subtracted spectra between the carbon black and HOPG, (carbon black) - (HOPG), show double-peak structures on both sides of the {pi}* peak. The lower-energy peak, denoted as the 'pre-peak', in the subtracted spectra and the {pi}*/{sigma}* peak intensity ratio in the absorption spectra clearly depend on the specific surface area by nitrogen adsorption (NSA). Therefore,more » it is concluded that the pre-peak intensity and the {pi}*/{sigma}* ratio reflect the local graphitic structure of carbon black.« less

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.

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

PubMed

Soares, Aline Rodrigues; Nascentes, Clésia Cristina

2013-02-15

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

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.

Atomization from a tantalum surface in graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Gregoire, D. C.; Chakrabarti, C. L.

The mechanism of atom formation of U, V, Mo, Ni, Mn, Cu and Mg atomized from pyrolytic graphite and tantalum metal surfaces has been studied. The mechanism of atom formation for U from a graphite tube atomizer is reported for the first time. The peak absorbance for U and Cu is increased by factors of 59.7 and 2.0, respectively, whereas that of V, Mo and Ni is reduced by several orders of magnitude when they are atomized from a tantalum metal surface. The peak absorbance of Mn and Mg is not appreciably affected by the material of the atomization surface. Interaction of Mn and Mg with the graphite surface and formation of their refractory carbides was found to be negligible. Uranium forms a refractory carbide when heated from a graphite surface.

Materials Science Research Rack-1 (MSRR-1)

NASA Technical Reports Server (NTRS)

2001-01-01

This scale model depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Here the transparent furnace is extracted for servicing. Key elements are labeled in other images (0101754, 0101829, 0101830, and TBD).

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.

Speciation of organic and inorganic selenium in selenium-enriched rice by graphite furnace atomic absorption spectrometry after cloud point extraction.

PubMed

Sun, Mei; Liu, Guijian; Wu, Qianghua

2013-11-01

A new method was developed for the determination of organic and inorganic selenium in selenium-enriched rice by graphite furnace atomic absorption spectrometry detection after cloud point extraction. Effective separation of organic and inorganic selenium in selenium-enriched rice was achieved by sequentially extracting with water and cyclohexane. Under the optimised conditions, the limit of detection (LOD) was 0.08 μg L(-1), the relative standard deviation (RSD) was 2.1% (c=10.0 μg L(-1), n=11), and the enrichment factor for selenium was 82. Recoveries of inorganic selenium in the selenium-enriched rice samples were between 90.3% and 106.0%. The proposed method was successfully applied for the determination of organic and inorganic selenium as well as total selenium in selenium-enriched rice. Copyright © 2013 Elsevier Ltd. All rights reserved.

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.

A study of graphite-epoxy laminate failures due to high transverse shear strains using the multi-span-beam shear test procedure

NASA Technical Reports Server (NTRS)

Jegley, Dawn C.

1989-01-01

The multi-span-beam shear test procedure is used to study failure mechanisms in graphite-epoxy laminates due to high transverse shear strains induced by severe local bending deformations in test specimens. Results of a series of tests on specimens with a variety of stacking sequences, including some with adhesive interleaving, are presented. These results indicate that laminates with stacking sequences with several + or - 45 and 90 deg plies next to each other are more susceptible to failures due to high transverse shear strains than laminates with + or - 45 and 0 deg plies next to each other or with + or - 45 deg plies next to layers of adhesive interleaving. Results of these tests are compared with analytical results based on finite elements.

Non-graphite crucible for high temperature applications

DOEpatents

Holcombe, Cressie E.; Pfeiler, William A.

1996-01-01

A multi-piece crucible for high temperature applications comprises a tubular side wall member having a lip on the inside surface and a bottom member or members forming a container for containing a melt of a material during a high temperature melt-casting operations. The multi-piece design prevents cracking of the crucible or leakage of the melt from the crucible during the melt-casting operation. The lip of the tubular member supports the bottom member. The contacting surfaces where the lip of the tubular side wall member contacts the bottom member of the multi-piece crucible contains a ceramic sealing material. The ceramic sealing material forms a seal sufficient to prevent the melt of the material from leaking out of the multi-piece crucible during the melt-casting process. The multi-piece crucible is made of a material which is chemically inert to the melt and has structural integrity at the melting point temperature of the melt, or of a material coated with such a material. The multi-piece crucible is contained in a thermal can assembly of a high temperature induction furnace during a high temperature melt-casting operation. One embodiment of the multi-piece crucible comprises a tubular member having a vertical slot filled with a ceramic sealing material to provide expansion of the tubular member without cracking during the high temperature melt-casting operation.

Non-graphite crucible for high temperature applications

DOEpatents

Holcombe, C.E.; Pfeiler, W.A.

1996-01-09

A multi-piece crucible for high temperature applications comprises a tubular side wall member having a lip on the inside surface and a bottom member or members forming a container for containing a melt of a material during a high temperature melt-casting operations. The multi-piece design prevents cracking of the crucible or leakage of the melt from the crucible during the melt-casting operation. The lip of the tubular member supports the bottom member. The contacting surfaces where the lip of the tubular side wall member contacts the bottom member of the multi-piece crucible contains a ceramic sealing material. The ceramic sealing material forms a seal sufficient to prevent the melt of the material from leaking out of the multi-piece crucible during the melt-casting process. The multi-piece crucible is made of a material which is chemically inert to the melt and has structural integrity at the melting point temperature of the melt, or of a material coated with such a material. The multi-piece crucible is contained in a thermal can assembly of a high temperature induction furnace during a high temperature melt-casting operation. One embodiment of the multi-piece crucible comprises a tubular member having a vertical slot filled with a ceramic sealing material to provide expansion of the tubular member without cracking during the high temperature melt-casting operation. 9 figs.

Study on Damage Mechanism of Ductile Cast Iron Cooling Stave

NASA Astrophysics Data System (ADS)

Wang, Cui; Zhang, Jianliang; Zuo, Haibin; Dai, Bing

The damage mechanism of ductile cast iron cooling stave applied to No.4 blast furnace of Guofeng steel was analyzed through damage investigation in details, the damage causes: high-temperature gas flow erosion, wear of burden, high-temperature ablation, carburizing damage, improper operation on blast furnace, etc. were given out both in macroscopic and microscopic views. It can be obtained from metallographic diagrams that the diameter of graphite nodules increases, the number per unit area reduces, and roundness declines, successively, from cold to hot surface, which are not conducive to stave longevity. In summary, the material for staves manufacture should be better in comprehensive mechanical properties to prolong the service life, thus making blast furnace long campaign.

Enhancement of oxidation resistance of graphite foams by polymer derived-silicon carbide coating for concentrated solar power applications

DOE PAGES

Kim, T.; Singh, D.; Singh, M.

2015-05-01

Graphite foam with extremely high thermal conductivity has been investigated to enhance heat transfer of latent heat thermal energy storage (LHTES) systems. However, the use of graphite foam for elevated temperature applications (>600 °C) is limited due to poor oxidation resistance of graphite. In the present study, oxidation resistance of graphite foam coated with silicon carbide (SiC) was investigated. A pre-ceramic polymer derived coating (PDC) method was used to form a SiC coating on the graphite foams. Post coating deposition, the samples were analyzed by scanning electron microscopy and energy dispersive spectroscopy. The oxidation resistance of PDC-SiC coating was quantifiedmore » by measuring the weight of the samples at several measuring points. The experiments were conducted under static argon atmosphere in a furnace. After the experiments, oxidation rates (%/hour) were calculated to predict the lifetime of the graphite foams. The experimental results showed that the PDC-SiC coating could prevent the oxidation of graphite foam under static argon atmosphere up to 900 °C.« less

Elements of EAF automation processes

NASA Astrophysics Data System (ADS)

Ioana, A.; Constantin, N.; Dragna, E. C.

2017-01-01

Our article presents elements of Electric Arc Furnace (EAF) automation. So, we present and analyze detailed two automation schemes: the scheme of electrical EAF automation system; the scheme of thermic EAF automation system. The application results of these scheme of automation consists in: the sensitive reduction of specific consummation of electrical energy of Electric Arc Furnace, increasing the productivity of Electric Arc Furnace, increase the quality of the developed steel, increasing the durability of the building elements of Electric Arc Furnace.

Approximate analytical solution for induction heating of solid cylinders

DOE PAGES

Jankowski, Todd Andrew; Pawley, Norma Helen; Gonzales, Lindsey Michal; ...

2015-10-20

An approximate solution to the mathematical model for induction heating of a solid cylinder in a cylindrical induction coil is presented here. The coupled multiphysics model includes equations describing the electromagnetic field in the heated object, a heat transfer simulation to determine temperature of the heated object, and an AC circuit simulation of the induction heating power supply. A multiple-scale perturbation method is used to solve the multiphysics model. The approximate analytical solution yields simple closed-form expressions for the electromagnetic field and heat generation rate in the solid cylinder, for the equivalent impedance of the associated tank circuit, and formore » the frequency response of a variable frequency power supply driving the tank circuit. The solution developed here is validated by comparing predicted power supply frequency to both experimental measurements and calculated values from finite element analysis for heating of graphite cylinders in an induction furnace. The simple expressions from the analytical solution clearly show the functional dependence of the power supply frequency on the material properties of the load and the geometrical characteristics of the furnace installation. In conclusion, the expressions developed here provide physical insight into observations made during load signature analysis of induction heating.« less

Burner Rig in the Material and Stresses Building

NASA Image and Video Library

1969-11-21

A burner rig heats up a material sample in the Materials and Stresses Building at the National Aeronautics and Space Administration (NASA) Lewis Research Center. Materials technology is an important element in the successful development of advanced airbreathing and rocket propulsion systems. Different types of engines operate in different environments so an array of dependable materials is needed. NASA Lewis began investigating the characteristics of different materials shortly after World War II. In 1949 the materials group was expanded into its own division. The Lewis researchers sought to study and test materials in environments that simulate the environment in which they would operate. The Materials and Stresses Building, built in 1949, contained a number of laboratories to analyze the materials. They are subjected to high temperatures, high stresses, corrosion, irradiation, and hot gasses. The Physics of Solids Laboratory included a cyclotron, cloud chamber, helium cryostat, and metallurgy cave. The Metallographic Laboratory possessed six x-ray diffraction machines, two metalloscopes, and other equipment. The Furnace Room had two large induction machines, a 4500⁰ F graphite furnace, and heat treating equipment. The Powder Laboratory included 60-ton and 3000-ton presses. The Stresses Laboratory included stress rupture machines, fatigue machines, and tensile strength machines.

LSSA large area silicon sheet task continuous Czochralski process development

NASA Technical Reports Server (NTRS)

Rea, S. N.

1978-01-01

A Czochralski crystal growing furnace was converted to a continuous growth facility by installation of a premelter to provide molten silicon flow into the primary crucible. The basic furnace is operational and several trial crystals were grown in the batch mode. Numerous premelter configurations were tested both in laboratory-scale equipment as well as in the actual furnace. The best arrangement tested to date is a vertical, cylindrical graphite heater containing small fused silicon test tube liner in which the incoming silicon is melted and flows into the primary crucible. Economic modeling of the continuous Czochralski process indicates that for 10 cm diameter crystal, 100 kg furnace runs of four or five crystals each are near-optimal. Costs tend to asymptote at the 100 kg level so little additional cost improvement occurs at larger runs. For these conditions, crystal cost in equivalent wafer area of around $20/sq m exclusive of polysilicon and slicing was obtained.

CdZnTe substrate impurities and their effects on liquid phase epitaxy HgCdTe

NASA Astrophysics Data System (ADS)

Tower, J. P.; Tobin, S. P.; Kestigian, M.; Norton, P. W.; Bollong, A. B.; Schaake, H. F.; Ard, C. K.

1995-05-01

Impurity levels were tracked through the stages of substrate and liquid phase epitaxy (LPE) layer processing to identify sources of elements which degrade infrared photodetector performance. Chemical analysis by glow discharge mass spectrometry and Zeeman corrected graphite furnace atomic absorption effectively showed the levels of impurities introduced into CdZnTe substrate material from the raw materials and the crystal growth processes. A new purification process (in situ distillation zone refining) for raw materials was developed, resulting in improved CdZnTe substrate purity. Substrate copper contamination was found to degrade the LPE layer and device electrical properties, in the case of lightly doped HgCdTe. Anomalous HgCdTe carrier type conversion was correlated to certain CdZnTe and CdTe substrate ingots.

High-purity silicon for solar cell applications

NASA Technical Reports Server (NTRS)

Dosaj, V. D.; Hunt, L. P.; Schei, A.

1978-01-01

The article discusses the production of solar cells from high-purity silicon. The process consists of reducing the level of impurities in the raw materials, preventing material contamination before and after entering the furnace, and performing orders-of-magnitude reduction of metal impurity concentrations. The high-purity raw materials are considered with reference to carbon reductants, silica, and graphite electrodes. Attention is also given to smelting experiments used to demonstrate, in an experimental-scale furnace, the production of high-purity SoG-Si. It is found that high-purity silicon may be produced from high-purity quartz and chemically purified charcoal in a 50-kVA arc furnace. The major contamination source is shown to be impurities from the carbon reducing materials.

A multi-zone muffle furnace design

NASA Technical Reports Server (NTRS)

Rowe, Neil D.; Kisel, Martin

1993-01-01

A Multi-Zone Muffle-Tube Furnace was designed, built, and tested for the purpose of providing an in-house experience base with tubular furnaces for materials processing in microgravity. As such, it must not only provide the desired temperatures and controlled thermal gradients at several discrete zones along its length but must also be capable of sustaining the rigors of a Space Shuttle launch. The furnace is insulated to minimize radial and axial heat losses. It is contained in a water-cooled enclosure for purposes of dissipating un-wanted residual heat, keeping the outer surfaces of the furnace at a 'touch-safe' temperature, and providing a rugged housing. This report describes the salient features of the furnace, testing procedures and results, and concluding remarks evaluating the overall design.

Temperature and flow fields in samples heated in monoellipsoidal mirror furnaces

NASA Astrophysics Data System (ADS)

Rivas, D.; Haya, R.

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

Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Peng, Jin-feng; Liu, Rui; Liu, Jing-fu; He, Bin; Hu, Xia-lin; Jiang, Gui-bin

2007-05-01

A new procedure, based on hollow fiber supported liquid membrane preconcentration coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection, was developed for the determination of trace Cd in seawater samples. With 1-octanol that contained a mixture of dithizone (carrier) and oleic acid immobilized in the pores of the polypropylene hollow fiber as a liquid membrane, Cd was selectively extracted from water samples into 0.05 M HNO 3 that filled the lumen of the hollow fiber as a stripping solution. The main extraction related parameters were optimized, and the effects of salinity and some coexisting interferants were also evaluated. Under the optimum extraction conditions, an enrichment factor of 387 was obtained for a 100-mL sample solution. In combination with graphite furnace atomic absorption spectrometry, a very low detection limit (0.8 ng L - 1 ) and a relative standard deviation (2.5% at 50 ng L - 1 level) were achieved. Five seawater samples were analyzed by the proposed method without dilution, with detected Cd concentration in the range of 56.4-264.8 ng L - 1 and the relative spiked recoveries over 89%. For comparison, these samples were also analyzed by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method after a 10-fold dilution for matrix effect elimination. Statistical analysis with a one-way ANOVA shows no significant differences (at 0.05 level) between the results obtained by the proposed and ICP-MS methods. Additionally, analysis of certified reference materials (GBW (E) 080040) shows good agreement with the certified value. These results indicate that this present method is very sensitive and reliable, and can effectively eliminate complex matrix interferences in seawater samples.

Development of a certified reference material (NMIJ CRM 7531-a) for the determination of trace cadmium and other elements in brown rice flour.

PubMed

Miyashita, Shin-ichi; Inagaki, Kazumi; Narukawa, Tomohiro; Zhu, Yanbei; Kuroiwa, Takayoshi; Hioki, Akiharu; Chiba, Koichi

2012-01-01

A certified reference material (CRM) for trace cadmium and other elements in brown rice flour was developed at the National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder after drying and frozen pulverization of fresh brown rice obtained from a Japanese domestic market. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), ICP high-resolution mass spectrometry, isotope-dilution ICP-MS, ICP optical emission spectrometry, and graphite-furnace atomic-absorption spectrometry. Property values were provided for six elements (Mn, Fe, Cu, Zn, As, and Cd). The concentration range of the property values was from 0.280 mg kg(-1) of As to 31.8 mg kg(-1) of Zn. The combined relative standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, characterization, difference among analytical methods, dry-mass correction factor, and calibration standard. The range of the relative combined standard uncertainties was from 1.1% of Zn to 1.6% of As.

Direct determination of trace refractory elements in human serum by ETV-ICP-MS with in-situ matrix removal.

PubMed

Li, Shengqing; Hu, Bin; Jiang, Zucheng; Chen, Rui

2004-08-01

A method for in-situ removal of matrix is proposed for direct determination of trace refractory elements in human serum by ETV-ICP-MS with the use of poly(tetrafluoroethylene) (PTFE) as fluorinating reagent. Attention has been paid to investigating the vaporization behavior both of refractory elements of interest and of matrix elements (Na, K, Ca, Mg, Cl, S, and P) in a graphite furnace with the PTFE modifier present or not. It was shown that potential interferences from the organic and inorganic matrices in the serum sample could be eliminated or reduced to a negligible level by appropriate dilution of the serum and deliberate optimization of the ETV temperature program. The proposed method has been applied to the direct simultaneous determination of V, Cr, Mo, Ba, La, Ce, and W in human serum. The limits of detection for fivefold diluted serum were 0.18 (V), 0.229 (Cr), 0.050 (Mo), 0.328 (Ba), 0.031 (La), 0.038 (Ce), and 0.019 ng mL(-1) (W), respectively, and the relative standard deviations of the method were in the range 4-15% (2 ng mL(-1) in serum, n=3).

The Nuclear Cryogenic Propulsion Stage

NASA Technical Reports Server (NTRS)

Houts, Michael G.; Kim, Tony; Emrich, William J.; Hickman, Robert R.; Broadway, Jeramie W.; Gerrish, Harold P.; Belvin, Anthony D.; Borowski, Stanley K.; Scott, John H.

2014-01-01

Nuclear Thermal Propulsion (NTP) development efforts in the United States have demonstrated the technical viability and performance potential of NTP systems. For example, Project Rover (1955 - 1973) completed 22 high power rocket reactor tests. Peak performances included operating at an average hydrogen exhaust temperature of 2550 K and a peak fuel power density of 5200 MW/m3 (Pewee test), operating at a thrust of 930 kN (Phoebus-2A test), and operating for 62.7 minutes in a single burn (NRX-A6 test). Results from Project Rover indicated that an NTP system with a high thrust-to-weight ratio and a specific impulse greater than 900 s would be feasible. Excellent results were also obtained by the former Soviet Union. Although historical programs had promising results, many factors would affect the development of a 21st century nuclear thermal rocket (NTR). Test facilities built in the US during Project Rover no longer exist. However, advances in analytical techniques, the ability to utilize or adapt existing facilities and infrastructure, and the ability to develop a limited number of new test facilities may enable affordable development, qualification, and utilization of a Nuclear Cryogenic Propulsion Stage (NCPS). Bead-loaded graphite fuel was utilized throughout the Rover/NERVA program, and coated graphite composite fuel (tested in the Nuclear Furnace) and cermet fuel both show potential for even higher performance than that demonstrated in the Rover/NERVA engine tests.. NASA's NCPS project was initiated in October, 2011, with the goal of assessing the affordability and viability of an NCPS. FY 2014 activities are focused on fabrication and test (non-nuclear) of both coated graphite composite fuel elements and cermet fuel elements. Additional activities include developing a pre-conceptual design of the NCPS stage and evaluating affordable strategies for NCPS development, qualification, and utilization. NCPS stage designs are focused on supporting human Mars missions. The NCPS is being designed to readily integrate with the Space Launch System (SLS). A wide range of strategies for enabling affordable NCPS development, qualification, and utilization should be considered. These include multiple test and demonstration strategies (both ground and in-space), multiple potential test sites, and multiple engine designs. Two potential NCPS fuels are currently under consideration - coated graphite composite fuel and tungsten cermet fuel. During 2014 a representative, partial length (approximately 16") coated graphite composite fuel element with prototypic depleted uranium loading is being fabricated at Oak Ridge National Laboratory (ORNL). In addition, a representative, partial length (approximately 16") cermet fuel element with prototypic depleted uranium loading is being fabricated at Marshall Space Flight Center (MSFC). During the development process small samples (approximately 3" length) will be tested in the Compact Fuel Element Environmental Tester (CFEET) at high temperature (approximately 2800 K) in a hydrogen environment to help ensure that basic fuel design and manufacturing process are adequate and have been performed correctly. Once designs and processes have been developed, longer fuel element segments will be fabricated and tested in the Nuclear Thermal Rocket Element Environmental Simulator (NTREE) at high temperature (approximately 2800 K) and in flowing hydrogen.

[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.

Analysis of beryllium and depleted uranium: An overview of detection methods in aerosols and soils

DOE Office of Scientific and Technical Information (OSTI.GOV)

Camins, I.; Shinn, J.H.

We conducted a survey of commercially available methods for analysis of beryllium and depleted uranium in aerosols and soils to find a reliable, cost-effective, and sufficiently precise method for researchers involved in environmental testing at the Yuma Proving Ground, Yuma, Arizona. Criteria used for evaluation include cost, method of analysis, specificity, sensitivity, reproducibility, applicability, and commercial availability. We found that atomic absorption spectrometry with graphite furnace meets these criteria for testing samples for beryllium. We found that this method can also be used to test samples for depleted uranium. However, atomic absorption with graphite furnace is not as sensitive amore » measurement method for depleted uranium as it is for beryllium, so we recommend that quality control of depleted uranium analysis be maintained by testing 10 of every 1000 samples by neutron activation analysis. We also evaluated 45 companies and institutions that provide analyses of beryllium and depleted uranium. 5 refs., 1 tab.« less

High temperature electrically conducting ceramic heating element and control system

NASA Technical Reports Server (NTRS)

Halbach, C. R.; Page, R. J.

1975-01-01

Improvements were made in both electrode technology and ceramic conductor quality to increase significantly the lifetime and thermal cycling capability of electrically conducting ceramic heater elements. These elements were operated in vacuum, inert and reducing environments as well as oxidizing atmospheres adding to the versatility of the conducting ceramic as an ohmic heater. Using stabilized zirconia conducting ceramic heater elements, a furnace was fabricated and demonstrated to have excellent thermal response and cycling capability. The furnace was used to melt platinum-20% rhodium alloy (melting point 1904 C) with an isothermal ceramic heating element having a nominal working cavity size of 2.5 cm diameter by 10.0 cm long. The furnace was operated to 1940 C with the isothermal ceramic heating element. The same furnace structure was fitted with a pair of main heater elements to provide axial gradient temperature control over a working cavity length of 17.8 cm.

Removable preheater elements improve oxide induction furnace

NASA Technical Reports Server (NTRS)

Leipold, M. H.

1964-01-01

Heat and corrosion resistant preheater elements are used in oxide induction furnaces to raise the temperature to the level for conducting electricity. These preheater elements are then removed and the induction coil energized.

Heat Source Characterization In A TREAT Fuel Particle Using Coupled Neutronics Binary Collision Monte-Carlo Calculations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schunert, Sebastian; Schwen, Daniel; Ghassemi, Pedram

This work presents a multi-physics, multi-scale approach to modeling the Transient Test Reactor (TREAT) currently prepared for restart at the Idaho National Laboratory. TREAT fuel is made up of microscopic fuel grains (r ˜ 20µm) dispersed in a graphite matrix. The novelty of this work is in coupling a binary collision Monte-Carlo (BCMC) model to the Finite Element based code Moose for solving a microsopic heat-conduction problem whose driving source is provided by the BCMC model tracking fission fragment energy deposition. This microscopic model is driven by a transient, engineering scale neutronics model coupled to an adiabatic heating model. Themore » macroscopic model provides local power densities and neutron energy spectra to the microscpic model. Currently, no feedback from the microscopic to the macroscopic model is considered. TREAT transient 15 is used to exemplify the capabilities of the multi-physics, multi-scale model, and it is found that the average fuel grain temperature differs from the average graphite temperature by 80 K despite the low-power transient. The large temperature difference has strong implications on the Doppler feedback a potential LEU TREAT core would see, and it underpins the need for multi-physics, multi-scale modeling of a TREAT LEU core.« less

EVALUATION OF A FIELD TEST KIT FOR MONITORING LEAD IN DRINKING WATER.

EPA Science Inventory

This article describes a conceptual framework for designing evaluation studies of test kits for the analysis of significant drinking water constituents. A commercial test kit for the analysis of lead in tap waters was evaluated and compared with a standard graphite furnace atomic...

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.

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Silicon Sheet Growth Development for the Large Area Sheet Task of the Low Cost Solar Array Project. Heat Exchanger Method - Ingot Casting Fixed Abrasive Method - Multi-Wire Slicing

NASA Technical Reports Server (NTRS)

Schmid, F.; Khattak, C. P.

1978-01-01

Solar cells fabricated from HEM cast silicon yielded up to 15% conversion efficiencies. This was achieved in spite of using unpurified graphite parts in the HEM furnace and without optimization of material or cell processing parameters. Molybdenum retainers prevented SiC formation and reduced carbon content by 50%. The oxygen content of vacuum cast HEM silicon is lower than typical Czochralski grown silicon. Impregnation of 45 micrometers diamonds into 7.5 micrometers copper sheath showed distortion of the copper layer. However, 12.5 micrometers and 15 micrometers copper sheath can be impregnated with 45 micrometers diamonds to a high concentration. Electroless nickel plating of wires impregnated only in the cutting edge showed nickel concentration around the diamonds. This has the possibility of reducing kerf. The high speed slicer fabricated can achieve higher speed and longer stroke with vibration isolation.

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

Microgravity

NASA Image and Video Library

2001-06-05

This computer-generated image depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101830, and TBD).

Microgravity

NASA Image and Video Library

2001-06-05

This computer-generated image depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101829, 0101830).

Microgravity

NASA Image and Video Library

2001-06-05

This scale model depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101829, 0101830, and TBD).

Ethanol Consumption by Wistar Rat Dams Affects Selenium Bioavailability and Antioxidant Balance in Their Progeny

PubMed Central

Ojeda, María Luisa; Vázquez, Beatriz; Nogales, Fátima; Murillo, María Luisa; Carreras, Olimpia

2009-01-01

Ethanol consumption affects maternal nutrition, the mothers’ antioxidant balance and the future health of their progeny. Selenium (Se) is a trace element cofactor of the enzyme glutathione peroxidase (GPx). We will study the effect of ethanol on Se bioavailability in dams and in their progeny. We have used three experimental groups of dams: control, chronic ethanol and pair-fed; and three groups of pups. Se levels were measured by graphite-furnace atomic absorption spectrometry. Serum and hepatic GPx activity was determined by spectrometry. We have concluded that ethanol decreased Se retention in dams, affecting their tissue Se deposits and those of their offspring, while also compromising their progeny’s weight and oxidation balance. These effects of ethanol are caused by a reduction in Se intake and a direct alcohol-generated oxidation action. PMID:19742151

Coated metal sintering carriers for fuel cell electrodes

DOEpatents

Donelson, Richard; Bryson, E. S.

1998-01-01

A carrier for conveying components of a fuel cell to be sintered through a sintering furnace. The carrier comprises a metal sheet coated with a water-based carbon paint, the water-based carbon paint comprising water, powdered graphite, an organic binder, a wetting agent, a dispersing agent and a defoaming agent.

Distribution of radionuclides during melting of carbon steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thurber, W.C.; MacKinney, J.

1997-02-01

During the melting of steel with radioactive contamination, radionuclides may be distributed among the metal product, the home scrap, the slag, the furnace lining and the off-gas collection system. In addition, some radionuclides will pass through the furnace system and vent to the atmosphere. To estimate radiological impacts of recycling radioactive scrap steel, it is essential to understand how radionuclides are distributed within the furnace system. For example, an isotope of a gaseous element (e.g., radon) will exhaust directly from the furnace system into the atmosphere while a relatively non-volatile element (e.g., manganese) can be distributed among all the othermore » possible media. This distribution of radioactive contaminants is a complex process that can be influenced by numerous chemical and physical factors, including composition of the steel bath, chemistry of the slag, vapor pressure of the particular element of interest, solubility of the element in molten iron, density of the oxide(s), steel melting temperature and melting practice (e.g., furnace type and size, melting time, method of carbon adjustment and method of alloy additions). This paper discusses the distribution of various elements with particular reference to electric arc furnace steelmaking. The first two sections consider the calculation of partition ratios for elements between metal and slag based on thermodynamic considerations. The third section presents laboratory and production measurements of the distribution of various elements among slag, metal, and the off-gas collection system; and the final section provides recommendations for the assumed distribution of each element of interest.« less

Characterization of airborne and bulk particulate from iron and steel manufacturing facilities.

PubMed

Machemer, Steven D

2004-01-15

Characterization of airborne and bulk particulate material from iron and steel manufacturing facilities, commonly referred to as kish, indicated graphite flakes and graphite flakes associated with spherical iron oxide particles were unique particle characteristics useful in identifying particle emissions from iron and steel manufacturing. Characterization of airborne particulate material collected in receptor areas was consistent with multiple atmospheric release events of kish particles from the local iron and steel facilities into neighboring residential areas. Kish particles deposited in nearby residential areas included an abundance of graphite flakes, tens of micrometers to millimeters in size, and spherical iron oxide particles, submicrometer to tens of micrometers in size. Bulk kish from local iron and steel facilities contained an abundance of similar particles. Approximately 60% of blast furnace kish by volume consisted of spherical iron oxide particles in the respirable size range. Basic oxygen furnace kish contained percent levels of strongly alkaline components such as calcium hydroxide. In addition, concentrations of respirable Mn in airborne particulate in residential areas and at local iron and steel facilities were approximately 1.6 and 53 times the inhalation reference concentration of 0.05 microg/m3 for chronic inhalation exposure of Mn, respectively. Thus, airborne release of kish may pose potential respirable particulate, corrosive, or toxic hazards for human health and/or a corrosive hazard for property and the environment.

Essential and toxic metals in tea (Camellia sinensis) imported and produced in Ethiopia.

PubMed

Ashenef, Ayenew

2014-01-01

Sixteen samples of packed tea leaves (Camellia sinensis) were purchased from supermarkets in Addis Ababa, Ethiopia for metal analysis. Elements were measured by FAAS and graphite furnace atomic absorption spectrometer (GFAAS) employing external calibration curves. The levels in mg/kg dried weight basis varied from Cu: 4.7-12.9; Cd: 0.02-2.83; Pb: <0.01-2.29; Zn: 8.6-198.3; Mn: 81.7-962.2; Al: 3376.4-10,369.3; K: 7667.7-10,775; Li: 0.2-0.62; Ba: 9.4-1407.1; Mg: 1145.6-1834.1; Fe: 286.4-880.9; Ca: 1414.2-2646.0; Na: 147.1-557.7. Levels of exposure to the investigated metals by drinking tea were checked with the recommended daily allowance (RDA) of the WHO/FAO. Considering the average daily consumption rate of tea alone, the possible daily intakes of Al, Ba and Mn surpass the amenability to the side effects associated with these elements like Alzheimer's disease, kidney damage and Parkinson's disease, respectively, for which drinking tea should cause awareness. The other investigated elements are in the acceptable range.

Catalytic Graphitization of Coal-Based Carbon Materials with Light Rare Earth Elements.

PubMed

Wang, Rongyan; Lu, Guimin; Qiao, Wenming; Yu, Jianguo

2016-08-30

The catalytic graphitization mechanism of coal-based carbon materials with light rare earth elements was investigated using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, selected-area electron diffraction, and high-resolution transmission electron microscopy. The interface between light rare earth elements and carbon materials was carefully observed, and two routes of rare earth elements catalyzing the carbon materials were found: dissolution-precipitation and carbide formation-decomposition. These two simultaneous processes certainly accelerate the catalytic graphitization of carbon materials, and light rare earth elements exert significant influence on the microstructure and thermal conductivity of graphite. Moreover, by virtue of praseodymium (Pr), it was found that a highly crystallographic orientation of graphite was induced and formed, which was reasonably attributed to the similar arrangements of the planes perpendicular to (001) in both graphite and Pr crystals. The interface between Pr and carbon was found to be an important factor for the orientation of graphite structure.

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

NASA Astrophysics Data System (ADS)

Rovnaník, P.; Míková, M.; Kusák, I.

2017-10-01

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

Determination of mineral, trace element, and pesticide levels in honey samples originating from different regions of Malaysia compared to manuka honey.

PubMed

Moniruzzaman, Mohammed; Chowdhury, Muhammed Alamgir Zaman; Rahman, Mohammad Abdur; Sulaiman, Siti Amrah; Gan, Siew Hua

2014-01-01

The present study was undertaken to determine the content of six minerals, five trace elements, and ten pesticide residues in honeys originating from different regions of Malaysia. Calcium (Ca), magnesium (Mg), iron (Fe), and zinc (Zn) were analyzed by flame atomic absorption spectrometry (FAAS), while sodium (Na) and potassium (K) were analyzed by flame emission spectrometry (FAES). Trace elements such as arsenic (As), lead (Pb), cadmium (Cd), copper (Cu), and cobalt (Co) were analyzed by graphite furnace atomic absorption spectrometry (GFAAS) following the microwave digestion of honey. High mineral contents were observed in the investigated honeys with K, Na, Ca, and Fe being the most abundant elements (mean concentrations of 1349.34, 236.80, 183.67, and 162.31 mg/kg, resp.). The concentrations of the trace elements were within the recommended limits, indicating that the honeys were of good quality. Principal component analysis reveals good discrimination between the different honey samples. The pesticide analysis for the presence of organophosphorus and carbamates was performed by high performance liquid chromatography (HPLC). No pesticide residues were detected in any of the investigated honey samples, indicating that the honeys were pure. Our study reveals that Malaysian honeys are rich sources of minerals with trace elements present within permissible limits and that they are free from pesticide contamination.

Determination of Mineral, Trace Element, and Pesticide Levels in Honey Samples Originating from Different Regions of Malaysia Compared to Manuka Honey

PubMed Central

Moniruzzaman, Mohammed; Chowdhury, Muhammed Alamgir Zaman; Rahman, Mohammad Abdur; Sulaiman, Siti Amrah; Gan, Siew Hua

2014-01-01

The present study was undertaken to determine the content of six minerals, five trace elements, and ten pesticide residues in honeys originating from different regions of Malaysia. Calcium (Ca), magnesium (Mg), iron (Fe), and zinc (Zn) were analyzed by flame atomic absorption spectrometry (FAAS), while sodium (Na) and potassium (K) were analyzed by flame emission spectrometry (FAES). Trace elements such as arsenic (As), lead (Pb), cadmium (Cd), copper (Cu), and cobalt (Co) were analyzed by graphite furnace atomic absorption spectrometry (GFAAS) following the microwave digestion of honey. High mineral contents were observed in the investigated honeys with K, Na, Ca, and Fe being the most abundant elements (mean concentrations of 1349.34, 236.80, 183.67, and 162.31 mg/kg, resp.). The concentrations of the trace elements were within the recommended limits, indicating that the honeys were of good quality. Principal component analysis reveals good discrimination between the different honey samples. The pesticide analysis for the presence of organophosphorus and carbamates was performed by high performance liquid chromatography (HPLC). No pesticide residues were detected in any of the investigated honey samples, indicating that the honeys were pure. Our study reveals that Malaysian honeys are rich sources of minerals with trace elements present within permissible limits and that they are free from pesticide contamination. PMID:24982869

Coated metal sintering carriers for fuel cell electrodes

DOEpatents

Donelson, R.; Bryson, E.S.

1998-11-10

A carrier is described for conveying components of a fuel cell to be sintered through a sintering furnace. The carrier comprises a metal sheet coated with a water-based carbon paint, the water-based carbon paint comprising water, powdered graphite, an organic binder, a wetting agent, a dispersing agent and a defoaming agent.

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

PubMed

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

2009-11-11

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

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.

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.

Several methods to determine heavy metals in the human brain

NASA Astrophysics Data System (ADS)

Andrási, Erzsébet; Igaz, Sarolta; Szoboszlai, Norbert; Farkas, Éva; Ajtony, Zsolt

1999-05-01

The determination of naturally occurring heavy metals in various parts of the human brain is discussed. The patients had no diseases in their central nervous systems (five individuals, mean age 70 years). Twenty brain parts were selected from both hemispheres. The analysis was carried out by graphite furnace atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis methods. Accuracy and precision of the applied techniques were tested by using standard reference materials. Two digestion methods were used to dissolve the brain samples for ICP-AES and GF-AAS. One was performed in a Parr-bomb and the second in a microwave oven. The present results show a non-homogeneous distribution of the essential elements (Cu, Fe, Mn, Zn) in normal human brain. Corresponding regions in both hemispheres showed an almost identical concentration of these elements. In the case of toxic elements (Pb, Cd) an average value in different brain regions can not be established because of the high variability of individual data. This study indicates that beside differences in Pb and Cd intake with foods or cigarette smoke inhalation, the main factors of the high inter-individual variability of these element concentrations in human brain parts may be a marked difference in individual elimination or accumulation capabilities.

Microwave plasma monitoring system for the elemental composition analysis of high temperature process streams

DOEpatents

Woskov, Paul P.; Cohn, Daniel R.; Titus, Charles H.; Surma, Jeffrey E.

1997-01-01

Microwave-induced plasma for continuous, real time trace element monitoring under harsh and variable conditions. The sensor includes a source of high power microwave energy and a shorted waveguide made of a microwave conductive, high temperature capability refractory material communicating with the source of the microwave energy to generate a plasma. The high power waveguide is constructed to be robust in a hot, hostile environment. It includes an aperture for the passage of gases to be analyzed and a spectrometer is connected to receive light from the plasma. Provision is made for real time in situ calibration. The spectrometer disperses the light, which is then analyzed by a computer. The sensor is capable of making continuous, real time quantitative measurements of desired elements, such as the heavy metals lead and mercury. The invention may be incorporated into a high temperature process device and implemented in situ for example, such as with a DC graphite electrode plasma arc furnace. The invention further provides a system for the elemental analysis of process streams by removing particulate and/or droplet samples therefrom and entraining such samples in the gas flow which passes through the plasma flame. Introduction of and entraining samples in the gas flow may be facilitated by a suction pump, regulating gas flow, gravity or combinations thereof.

Arc melting and homogenization of ZrC and ZrC + B alloys

NASA Technical Reports Server (NTRS)

Darolia, R.; Archbold, T. F.

1973-01-01

A description is given of the methods used to arc-melt and to homogenize near-stoichiometric ZrC and ZrC-boron alloys, giving attention to the oxygen contamination problem. The starting material for the carbide preparation was ZrC powder with an average particle size of 4.6 micron. Pellets weighing approximately 3 g each were prepared at room temperature from the powder by the use of an isostatic press operated at 50,000 psi. These pellets were individually melted in an arc furnace containing a static atmosphere of purified argon. A graphite resistance furnace was used for the homogenization process.

Preliminary science report on the directional solidification of hypereutectic cast iron during KC-135 low-G maneuvers

NASA Technical Reports Server (NTRS)

Curreri, P. A.; Stefanescu, D. M.; Hendrix, J. C.

1983-01-01

An ADSS-P directional solidification furnace was reconfigured for operation on the KC-135 low-g aircraft. The system offers many advantages over quench ingot methods for study of the effects of sedimentation and convection on alloy formation. The directional sodification furnace system was first flown during the September 1982 series of flights. The microstructure of the hypereutectic cast iron sample solidified on one of these flights suggests a low-g effect on graphite morphology. Further experiments are needed to ascertain that this effect is due to low-gravity and to deduce which of the possible mechanisms is responsible for it.

Materials Science Research Rack-1 (MSRR-1)

NASA Technical Reports Server (NTRS)

2001-01-01

This computer-generated image depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101829, 0101830, and TBD).

Materials Science Research Rack-1 (MSRR-1)

NASA Technical Reports Server (NTRS)

2001-01-01

This computer-generated image depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101830, and TBD).

Materials Science Research Rack-1 (MSRR-1)

NASA Technical Reports Server (NTRS)

2001-01-01

This scale model depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101829, 0101830, and TBD).

Materials Science Research Rack-1 (MSRR-1)

NASA Technical Reports Server (NTRS)

2001-01-01

This computer-generated image depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101829, 0101830).

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.

Seasonal investigation of trace element contents in commercially valuable fish species from the Black sea, Turkey.

PubMed

Mendil, Durali; Demirci, Zafer; Tuzen, Mustafa; Soylak, Mustafa

2010-03-01

Fish species (Sarda sarda, Mulus barbatus ponticus, Trachurus trachurus and Merlangius merlangus) were collected from the Black sea, Turkey between 2008 and 2009 (spring, summer, autumn and winter). The samples were analyzed using flame and graphite furnace atomic absorption spectrometry after microwave digestion. The maximum metal concentrations were found to be as 25.5-41.4 microg/g (Fe), 17.8-25.7 microg/g (Zn), 0.28-0.64 microg/g (Pb), 0.64-0.99 microg/g (Cr), 1.3-3.6 microg/g (Mn), 1.4-1.9 microg/g (Cu), 0.18-0.35 microg/g (Cd) and 0.25-0.42 microg/g (Co) for fish species. The concentration of trace metals in samples is depended on fish species. Some species is accumulated trace metals at high ratio. Trace element levels in analyzed fish species were acceptable to human consumption at nutritional and toxic levels. The levels of lead and cadmium in fish samples were higher than the recommended legal limits. Copyright (c) 2009 Elsevier Ltd. All rights reserved.

Direct sampling graphite furnace atomic absorption spectrometry - feasibility of Na and K determination in desalted crude oil

NASA Astrophysics Data System (ADS)

Seeger, Tassia S.; Machado, Eduarda Q.; Flores, Erico M. M.; Mello, Paola A.; Duarte, Fabio A.

2018-03-01

In this study, Na and K were determined in desalted crude oil by direct sampling graphite furnace atomic absorption spectrometry (DS-GF AAS), with the use of a Zeeman-effect background correction system with variable magnetic field. The analysis was performed in low and high sensitivity conditions. Sodium determination was performed in two low-sensitivity conditions: 1) main absorption line (589.0 nm), gas stop flow during the atomization step and 3-field dynamic mode (0.6-0.8 T); and 2) secondary absorption line (330.3 nm), gas stop flow during the atomization and 2-field mode (0.8 T). In K determination, some parameters, such as high-sensitivity mode, main absorption line (766.5 nm), gas stop flow during the atomization and 2-field mode (0.8 T), were used. Suitability of chemical modifiers, such as Pd and W-Ir was also evaluated. The heating program for Na and K was based on the pyrolysis and atomization curves. Calibration was performed by aqueous standards. Accuracy was evaluated by the analysis of Green Petroleum Coke (SRM NIST 2718) and Trace Elements in Fuel Oil (SRM NIST 1634c). Recovery tests were also performed and results were compared with those obtained by GF AAS after crude oil digestion by microwave-assisted digestion. The characteristic mass of Na was 17.1 pg and 0.46 ng in conditions 1 and 2, respectively, while the one of K was 1.4 pg. Limits of detection and quantification by DS-GF AAS were 30 and 40 ng g-1 for Na and 3.2 and 4.2 ng g-1 for K, respectively. Sodium and K were determined in three crude oil samples with API density ranging from 20.9 to 28.0. Sodium and K concentration ranged from 1.5 to 73 μg g-1 and from 23 to 522 ng g-1, respectively.

Stable aqueous dispersions of functionalized multi-layer graphene by pulsed underwater plasma exfoliation of graphite

NASA Astrophysics Data System (ADS)

Meyer-Plath, Asmus; Beckert, Fabian; Tölle, Folke J.; Sturm, Heinz; Mülhaupt, Rolf

2016-02-01

A process was developed for graphite particle exfoliation in water to stably dispersed multi-layer graphene. It uses electrohydraulic shockwaves and the functionalizing effect of solution plasma discharges in water. The discharges were excited by 100 ns high voltage pulsing of graphite particle chains that bridge an electrode gap. The underwater discharges allow simultaneous exfoliation and chemical functionalization of graphite particles to partially oxidized multi-layer graphene. Exfoliation is caused by shockwaves that result from rapid evaporation of carbon and water to plasma-excited gas species. Depending on discharge energy and locus of ignition, the shockwaves cause stirring, erosion, exfoliation and/or expansion of graphite flakes. The process was optimized to produce long-term stable aqueous dispersions of multi-layer graphene from graphite in a single process step without requiring addition of intercalants, surfactants, binders or special solvents. A setup was developed that allows continuous production of aqueous dispersions of flake size-selected multi-layer graphenes. Due to the well-preserved sp2-carbon structure, thin films made from the dispersed graphene exhibited high electrical conductivity. Underwater plasma discharge processing exhibits high innovation potential for morphological and chemical modifications of carbonaceous materials and surfaces, especially for the generation of stable dispersions of two-dimensional, layered materials.

Simultaneous determination of iron, cadmium, zinc, copper, nickel, lead, and uranium in seawater by stable isotope dilution spark source mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mykytiuk, A.P.; Russell, D.S.; Sturgeon, R.E.

Trace concentrations (ng/mL) of Fe, Cd, Zn, Cu, Ni, Pb, U, and Co have been determined in seawater by stable isotope dilution spark source mass spectrometry. The seawater samples were preconcentrated on the ion exchanger Chelex-100 and the concentrate was evaporated on a graphite or silver electrode. The results are compared with those obtained by graphite furnace atomic absorption spectrometry and inductively coupled plasma emission spectrometry. The technique avoids the use of calibration standards and is capable of producing results in cases where the analyte is only partially recovered. 2 tables.

Manufacturing processes for fabricating graphite/PMR 15 polyimide structural elements

NASA Technical Reports Server (NTRS)

Sheppard, C. H.; Hoggatt, J. T.; Symonds, W. A.

1979-01-01

Investigations were conducted to obtain commercially available graphite/PMR-15 polyimide prepreg, develop an autoclave manufacturing process, and demonstrate the process by manufacturing structural elements. Controls were established on polymer, prepreg, composite fabrication, and quality assurance, Successful material quality control and processes were demonstrated by fabricating major structural elements including flat laminates, hat sections, I beam sections, honeycomb sandwich structures, and molded graphite reinforced fittings. Successful fabrication of structural elements and simulated section of the space shuttle aft body flap shows that the graphite/PMR-15 polyimide system and the developed processes are ready for further evaluation in flight test hardware.

Thermodynamic Simulation of Equilibrium Composition of Reaction Products at Dehydration of a Technological Channel in a Uranium-Graphite Reactor

NASA Astrophysics Data System (ADS)

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

2018-01-01

The problems of accumulation of nuclear fuel spills in the graphite stack in the course of operation of uranium-graphite nuclear reactors are considered. The results of thermodynamic analysis of the processes in the graphite stack at dehydration of a technological channel, fuel element shell unsealing and migration of fission products, and activation of stable nuclides in structural elements of the reactor and actinides inside the graphite moderator are given. The main chemical reactions and compounds that are produced in these modes in the reactor channel during its operation and that may be hazardous after its shutdown and decommissioning are presented. Thermodynamic simulation of the equilibrium composition is performed using the specialized code TERRA. The results of thermodynamic simulation of the equilibrium composition in different cases of technological channel dehydration in the course of the reactor operation show that, if the temperature inside the active core of the nuclear reactor increases to the melting temperature of the fuel element, oxides and carbides of nuclear fuel are produced. The mathematical model of the nonstationary heat transfer in a graphite stack of a uranium-graphite reactor in the case of the technological channel dehydration is presented. The results of calculated temperature evolution at the center of the fuel element, the replaceable graphite element, the air gap, and in the surface layer of the block graphite are given. The numerical results show that, in the case of dehydration of the technological channel in the uranium-graphite reactor with metallic uranium, the main reaction product is uranium dioxide UO2 in the condensed phase. Low probability of production of pyrophoric uranium compounds (UH3) in the graphite stack is proven, which allows one to disassemble the graphite stack without the risk of spontaneous graphite ignition in the course of decommissioning of the uranium-graphite nuclear reactor.

Materials Science Research Rack-1 (MSRR-1)

NASA Technical Reports Server (NTRS)

2001-01-01

This scale model depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101829, 0101830, and TBD). This image is from a digital still camera; higher resolution is not available.

Microgravity

NASA Image and Video Library

2001-06-05

This scale model depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101829, and TBD). This composite is from a digital still camera; higher resolution is not available.

Microgravity

NASA Image and Video Library

2001-06-05

This scale model depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101829, 0101830, and TBD). This image is from a digital still camera; higher resolution is not available.

Materials Science Research Rack-1 (MSRR-1)

NASA Technical Reports Server (NTRS)

2001-01-01

This scale model depicts the Materials Science Research Rack-1 (MSRR-1) being developed by NASA's Marshall Space Flight Center and the European Space Agency (ESA) for placement in the Destiny laboratory module aboard the International Space Station. The rack is part of the plarned Materials Science Research Facility (MSRF) and is expected to include two furnace module inserts, a Quench Module Insert (being developed by NASA's Marshall Space Flight Center) to study directional solidification in rapidly cooled alloys and a Diffusion Module Insert (being developed by the European Space Agency) to study crystal growth, and a transparent furnace (being developed by NASA's Space Product Development program). Multi-user equipment in the rack is being developed under the auspices of NASA's Office of Biological and Physical Research (OBPR) and ESA. Key elements are labeled in other images (0101754, 0101829, and TBD). This composite is from a digital still camera; higher resolution is not available.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION AND MAINTENANCE OF THE PERKIN-ELMER ZEEMAN/5000 SYSTEM ATOMIC ABSORPTION SPECTROMETER (BCO-L-6.0)

EPA Science Inventory

The purpose of this SOP is to outline the start-up, calibration, operation, and maintenance procedures for the Perkin-Elmer 5000 atomic absorption spectrophotometer (PE 5000 AA), and the Perkin Elmer 5000 Zeeman graphite furnace atomic absorption spectrophotometer (PE 5000Z GFAA)...

Formation mechanism of the protective layer in a blast furnace hearth

NASA Astrophysics Data System (ADS)

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

2015-10-01

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

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

PubMed

Sun, Mei; Wu, Qianghua

2010-04-15

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

Effects of varying oxygen partial pressure on molten silicon-ceramic substrate interactions

NASA Technical Reports Server (NTRS)

Ownby, D. P.; Barsoum, M. W.

1980-01-01

The silicon sessile drop contact angle was measured on hot pressed silicon nitride, silicon nitride coated on hot pressed silicon nitride, silicon carbon coated on graphite, and on Sialon to determine the degree to which silicon wets these substances. The post-sessile drop experiment samples were sectioned and photomicrographs were taken of the silicon-substrate interface to observe the degree of surface dissolution and degradation. Of these materials, silicon did not form a true sessile drop on the SiC on graphite due to infiltration of the silicon through the SiC coating, nor on the Sialon due to the formation of a more-or-less rigid coating on the liquid silicon. The most wetting was obtained on the coated Si3N4 with a value of 42 deg. The oxygen concentrations in a silicon ribbon furnace and in a sessile drop furnace were measured using the protable thoria-yttria solid solution electrolyte oxygen sensor. Oxygen partial pressures of 10 to the minus 7 power atm and 10 to the minus 8 power atm were obtained at the two facilities. These measurements are believed to represent nonequilibrium conditions.

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.

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.

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. © 2013 Published by Elsevier B.V.

The level of elements and antioxidant activity of commercial dietary supplement formulations based on edible mushrooms.

PubMed

Stilinović, Nebojša; Škrbić, Biljana; Živančev, Jelena; Mrmoš, Nataša; Pavlović, Nebojša; Vukmirović, Saša

2014-12-01

Commercial preparations of Cordyceps sinensis, Ganoderma lucidum and Coprinus comatus mushroom marketed as healthy food supplements in Serbia were analyzed by atomic absorption spectrometry with a graphite furnace (GFAAS) for their element content. Antioxidant activity potential and total phenolics of the same mushrooms were determined. The element content of mushroom samples was in the range of 0.130-0.360 mg kg(-1) for lead (Pb), <0.03-0.46 mg kg(-1) for arsenic (As), 0.09-0.39 mg kg(-1) for cadmium (Cd), 98.14-989.18 mg kg(-1) for iron (Fe), 0.10-101.32 mg kg(-1) for nickel (Ni), 5.06-26.50 mg kg(-1) for copper (Cu), 0.20-0.70 mg kg(-1) for cobalt (Co), 1.74-136.33 mg kg(-1) for chromium (Cr) and 2.19-21.54 mg kg(-1) for manganese (Mn). In the tests for measuring the antioxidant activity, the methanolic extract of C. sinensis showed the best properties. The same was seen for the analysis of selected phenolic compounds; C. sinensis was found to have the highest content. Commercial preparations of C. sinensis and C. comatus can be considered to be safe and suitable food supplements included in well-balanced diets.

Qualitative and Quantitative Content Determination of Macro-Minor Elements in Bryonia Alba L. Roots using Flame Atomic Absorption Spectroscopy Technique.

PubMed

Karpiuk, Uliana Vladimirovna; Al Azzam, Khaldun Mohammad; Abudayeh, Zead Helmi Mahmoud; Kislichenko, Viktoria; Naddaf, Ahmad; Cholak, Irina; Yemelianova, Oksana

2016-06-01

To determine the elements in Bryonia alba L. roots, collected from the Crimean Peninsula region in Ukraine. Dry ashing was used as a flexible method and all elements were determined using atomic absorption spectrometry (AAS) equipped with flame and graphite furnace. The average concentrations of the determined elements, expressed as mg/100 g dry weight of the sample, were as follow: 13.000 for Fe, 78.000 for Si, 88.000 for P, 7.800 for Al, 0.130 for Mn, 105.000 for Mg, 0.030 for Pb, 0.052 for Ni, 0.030 for Mo, 210.000 for Ca, 0.130 for Cu, 5.200 for Zn, 13.000 for Na, 1170.000 for K, 0.780 for Sr, 0.030 for Co, 0.010 for Cd, 0.010 for As, and 0.010 for Hg. Toxic elements such as Cd and Pb were also found but at very low concentration. Among the analyzed elements, K was the most abundant followed by Ca, Mg, P, Si, Fe, Na, and Zn, whereas Hg, As, Cd, Co, Mo, and Pb were found in low concentration. The results suggest that the roots of Bryonia alba L. plant has potential medicinal property through their high element contents present. Moreover, it showed that the AAS method is a simple, fast, and reliable for the determination of elements in plant materials. The obtained results of the current study provide justification for the usage of such fruit in daily diet for nutrition and for medicinal usage in the treatment of various diseases.

Trace elements in sediments, blue spotted tilapia Oreochromis leucostictus (Trewavas, 1933) and its parasite Contracaecum multipapillatum from Lake Naivasha, Kenya, including a comprehensive health risk analysis.

PubMed

Otachi, Elick O; Körner, Wilfried; Avenant-Oldewage, Annemariè; Fellner-Frank, Christine; Jirsa, Franz

2014-06-01

This study presents the distribution of 15 major and trace elements in sediments and fish and their pericardial parasites from Lake Naivasha, Kenya. The lake is one of the few freshwater lakes in the Great Rift Valley and is under strong anthropogenic pressure mainly due to agricultural activities. Its fish provide a valuable protein source for approximately 100,000 people in the area. Fish and their parasites have been acknowledged as indicators of environmental quality due to their accumulation potential for both essential and nonessential trace elements. A total of 34 specimens of the blue spotted tilapia Oreochromis leucostictus and pooled samples of their pericardial parasite, the anisakid nematode Contracaecum multipapillatum (larvae 3), were examined. Element concentrations were determined by inductively coupled plasma-optical emission spectroscopy (ICP-OES) and graphite furnace atomic absorption spectrometry (GF-AAS). The concentrations of elements in the sediments reflected the geology of the area and did not point to pollution: none of the investigated trace elements, including Pb, Cd, Cu, and Zn, showed elevated values. In contrast, concentrations in the fish muscle were elevated for Li, Sr, Cd, and Zn, with high target hazard quotients (THQ > 0.1) indicating a potential health risk to the consumers of this fish. Fish liver showed significantly higher concentrations of the trace elements Fe, Mn, Cd, and Cu compared to the muscle and C. multipapillatum. In the parasite, Zn had the highest concentration, but the worms only minimally accumulated trace elements in relation to their fish host.

Multi-walled Carbon Nanotubes/Graphite Nanosheets Modified Glassy Carbon Electrode for the Simultaneous Determination of Acetaminophen and Dopamine.

PubMed

Zhang, Susu; He, Ping; Zhang, Guangli; Lei, Wen; He, Huichao

2015-01-01

Graphite nanosheets prepared by thermal expansion and successive sonication were utilized for the construction of a multi-walled carbon nanotubes/graphite nanosheets based amperometric sensing platform to simultaneously determine acetaminophen and dopamine in the presence of ascorbic acid in physiological conditions. The synergistic effect of multi-walled carbon nanotubes and graphite nanosheets catalyzed the electrooxidation of acetaminophen and dopamine, leading to a remarkable potential difference up to 200 mV. The as-prepared modified electrode exhibited linear responses to acetaminophen and dopamine in the concentration ranges of 2.0 × 10(-6) - 2.4 × 10(-4) M (R = 0.999) and 2.0 × 10(-6) - 2.0 × 10(-4) M (R = 0.998), respectively. The detection limits were down to 2.3 × 10(-7) M for acetaminophen and 3.5 × 10(-7) M for dopamine (S/N = 3). Based on the simple preparation and prominent electrochemical properties, the obtained multi-walled carbon nanotubes/graphite nanosheets modified electrode would be a good candidate for the determination of acetaminophen and dopamine without the interference of ascorbic acid.

The use of atomic spectroscopy in the pharmaceutical industry for the determination of trace elements in pharmaceuticals.

PubMed

Lewen, Nancy

2011-06-25

The subject of the analysis of various elements, including metals and metalloids, in the pharmaceutical industry has seen increasing importance in the last 10-15 years, as modern analytical instrumentation has afforded analysts with the opportunity to provide element-specific, accurate and meaningful information related to pharmaceutical products. Armed with toxicological data, compendial and regulatory agencies have revisited traditional approaches to the testing of pharmaceuticals for metals and metalloids, and analysts have begun to employ the techniques of atomic spectroscopy, such as flame- and graphite furnace atomic absorption spectroscopy (FAAS, Flame AA or FAA and GFAAS), inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and inductively coupled plasma-mass spectrometry (ICP-MS), to meet their analytical needs. Newer techniques, such as laser-induced breakdown spectroscopy (LIBS) and Laser Ablation ICP-MS (LAICP-MS) are also beginning to see wider applications in the analysis of elements in the pharmaceutical industry.This article will provide a perspective regarding the various applications of atomic spectroscopy in the analysis of metals and metalloids in drug products, active pharmaceutical ingredients (API's), raw materials and intermediates. The application of atomic spectroscopy in the analysis of metals and metalloids in clinical samples, nutraceutical, metabolism and pharmacokinetic samples will not be addressed in this work. Copyright © 2010 Elsevier B.V. All rights reserved.

Trace analysis of high-purity graphite by LA-ICP-MS.

PubMed

Pickhardt, C; Becker, J S

2001-07-01

Laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been established as a very efficient and sensitive technique for the direct analysis of solids. In this work the capability of LA-ICP-MS was investigated for determination of trace elements in high-purity graphite. Synthetic laboratory standards with a graphite matrix were prepared for the purpose of quantifying the analytical results. Doped trace elements, concentration 0.5 microg g(-1), in a laboratory standard were determined with an accuracy of 1% to +/- 7% and a relative standard deviation (RSD) of 2-13%. Solution-based calibration was also used for quantitative analysis of high-purity graphite. It was found that such calibration led to analytical results for trace-element determination in graphite with accuracy similar to that obtained by use of synthetic laboratory standards for quantification of analytical results. Results from quantitative determination of trace impurities in a real reactor-graphite sample, using both quantification approaches, were in good agreement. Detection limits for all elements of interest were determined in the low ng g(-1) concentration range. Improvement of detection limits by a factor of 10 was achieved for analyses of high-purity graphite with LA-ICP-MS under wet plasma conditions, because the lower background signal and increased element sensitivity.

GAS COOLED NUCLEAR REACTORS

DOEpatents

Long, E.; Rodwell, W.

1958-06-10

A gas-cooled nuclear reactor consisting of a graphite reacting core and reflector structure supported in a containing vessel is described. A gas sealing means is included for sealing between the walls of the graphite structure and containing vessel to prevent the gas coolant by-passing the reacting core. The reacting core is a multi-sided right prismatic structure having a pair of parallel slots around its periphery. The containing vessel is cylindrical and has a rib on its internal surface which supports two continuous ring shaped flexible web members with their radially innermost ends in sealing engagement within the radially outermost portion of the slots. The core structure is supported on ball bearings. This design permits thermal expansion of the core stracture and vessel while maintainirg a peripheral seal between the tvo elements.

THE FUEL ELEMENT GRAPHITE. Project DRAGON.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Graham, L.W.; Price, M.S.T.

1963-01-15

The main requirements of a fuel element graphite for reactors based on the Dragon concept are low transmission coefficient for fission products, dimensional stability under service conditions, high strength, high thermal conductivity, high purity, and high resistance to oxidation. Since conclusions reached in early 1960, a considerable amount of information has accumulated concerning the likely behaviour of graphites in high temperature reactor systems, particularly data on dimensional stability under irradiation. The influence of this new knowledge on the development of fuel element graphite with the Dragon Project is discussed in detail in the final section of this paper.

Trace element reference values in tissues from inhabitants of the European Community. III. The control of preanalytical factors in the biomonitoring of trace elements in biological fluids.

PubMed

Minoia, C; Pietra, R; Sabbioni, E; Ronchi, A; Gatti, A; Cavalleri, A; Manzo, L

1992-06-09

In the context of a programme concerning the determination of trace elements in body fluids and tissues to establish trace element reference values, research has been undertaken on the control of preanalytical factors in order to develop sufficiently accurate and precise guidelines to be applied in routine work by using techniques such as graphite furnace atomic absorption spectroscopy (GFAAS). Aspects investigated are related to the risk of contamination during blood collection and the use of anticoagulants; the risk of losses during storage and freeze-drying as well as the possible risk of contamination arising from trace elements in airborne particulates of the laboratory environment. For the analysis of Al, Ba, Cd, Co, Cr, Mn, Mo, Ni, Sb, W, V and Zn in blood, Teflon cannula is the method of choice. The anticoagulants do not introduce disturbing contaminations of Rb, Se, Zn, while contaminations were observed for Co, Cr, Mn. Radiotracers in 'metabolized form' (radiolabelled rat or rabbit tissues from animals administered with radioisotopes) show that samples stored for 1 month at -20 degrees C have no significant trace metal losses. Strict ambient air quality standard has to be respected (continuous monitoring) due to the possibility of element contaminations inside the laboratory. The use of matrix modifiers could represent a toxicological risk to the operators. Critical factors should be considered ('metal sheets') for each element in each matrix. For instance 27 factors for Cr in serum have been suggested.

Evaluation of dietary exposure to minerals, trace elements and heavy metals from the muscle tissue of the lionfish Pterois volitans (Linnaeus 1758).

PubMed

Hoo Fung, Leslie A; Antoine, Johann M R; Grant, Charles N; Buddo, Dayne St A

2013-10-01

Twenty-five samples of Pterois volitans caught in Jamaican waters were analyzed for 25 essential, non-essential and toxic elements using Graphite Furnace Atomic Absorption Spectrophotometry (GF-AAS), Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) and Instrumental Neutron Activation Analysis (INAA). The mean values for calcium (355 mg/kg), copper (107 μg/kg), iron (0.81 mg/kg), potassium (3481 mg/kg), magnesium (322 mg/kg), manganese (0.04 mg/kg), selenium (0.47 mg/kg), sodium (700 mg/kg) and zinc (4.46 mg/kg) were used to estimate dietary intake. The percentage contribution to provisional tolerable weekly intake for a 70 kg male and a 65 kg female were also estimated for the toxic elements arsenic (1.28% M, 1.38% F), cadmium (0.26% M. 0.28% F), mercury (3.85% M, 4.15% F) and lead (0.17% M, 0.18% F). To further assess the risk of mercury toxicity and the role of mitigation provided by selenium, selenium-mercury molar ratios were calculated for all samples. All samples were shown to have a molar excess of selenium. In addition the suggested selenium health benefit value was calculated, and was positive for all samples. It was concluded that P. volitans appears to contribute modestly to mineral and trace element nutrition, while not being a significant contributor to dietary exposure of toxic elements. Copyright © 2013 Elsevier Ltd. All rights reserved.

Monte Carlo simulation of electrothermal atomization on a desktop personal computer

NASA Astrophysics Data System (ADS)

Histen, Timothy E.; Güell, Oscar A.; Chavez, Iris A.; Holcombea, James A.

1996-07-01

Monte Carlo simulations have been applied to electrothermal atomization (ETA) using a tubular atomizer (e.g. graphite furnace) because of the complexity in the geometry, heating, molecular interactions, etc. The intense computational time needed to accurately model ETA often limited its effective implementation to the use of supercomputers. However, with the advent of more powerful desktop processors, this is no longer the case. A C-based program has been developed and can be used under Windows TM or DOS. With this program, basic parameters such as furnace dimensions, sample placement, furnace heating and kinetic parameters such as activation energies for desorption and adsorption can be varied to show the absorbance profile dependence on these parameters. Even data such as time-dependent spatial distribution of analyte inside the furnace can be collected. The DOS version also permits input of external temperaturetime data to permit comparison of simulated profiles with experimentally obtained absorbance data. The run-time versions are provided along with the source code. This article is an electronic publication in Spectrochimica Acta Electronica (SAE), the electronic section of Spectrochimica Acta Part B (SAB). The hardcopy text is accompanied by a diskette with a program (PC format), data files and text files.

Advanced techniques for determining long term compatibility of materials with propellants

NASA Technical Reports Server (NTRS)

Green, R. L.; Stebbins, J. P.; Smith, A. W.; Pullen, K. E.

1973-01-01

A method for the prediction of propellant-material compatibility for periods of time up to ten years is presented. Advanced sensitive measurement techniques used in the prediction method are described. These include: neutron activation analysis, radioactive tracer technique, and atomic absorption spectroscopy with a graphite tube furnace sampler. The results of laboratory tests performed to verify the prediction method are presented.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION, AND MAINTENANCE OF THE PERKIN-ELMER ZEEMAN/5000 SYSTEM ATOMIC ABSORPTION SPECTROPHOTOMETER (BCO-L-6.0)

EPA Science Inventory

The purpose of this SOP is to outline the start-up, calibration, operation, and maintenance procedures for the Perkin-Elmer 5000 atomic absorption spectrophotometer (PE 5000 AA), and the Perkin Elmer 5000 Zeeman graphite furnace atomic absorption spectrophotometer (PE 5000Z GFAA)...

Control of carbon balance in a silicon smelting furnace

DOEpatents

Dosaj, Vishu D.; Haines, Cathryn M.; May, James B.; Oleson, John D.

1992-12-29

The present invention is a process for the carbothermic reduction of silicon dioxide to form elemental silicon. Carbon balance of the process is assessed by measuring the amount of carbon monoxide evolved in offgas exiting the furnace. A ratio of the amount of carbon monoxide evolved and the amount of silicon dioxide added to the furnace is determined. Based on this ratio, the carbon balance of the furnace can be determined and carbon feed can be adjusted to maintain the furnace in carbon balance.

Efficient growth of HTS films with volatile elements

DOEpatents

Siegal, M.P.; Overmyer, D.L.; Dominguez, F.

1998-12-22

A system is disclosed for applying a volatile element-HTS layer, such as Tl-HTS, to a substrate in a multiple zone furnace, said method includes heating at higher temperature, in one zone of the furnace, a substrate and adjacent first source of Tl-HTS material, to sublimate Tl-oxide from the source to the substrate; and heating at lower temperature, in a separate zone of the furnace, a second source of Tl-oxide to replenish the first source of Tl-oxide from the second source. 3 figs.

The use of mosses as environmental metal pollution indicators.

PubMed

Aceto, Maurizio; Abollino, Ornella; Conca, Raffaele; Malandrino, Mery; Mentasti, Edoardo; Sarzanini, Corrado

2003-01-01

The possibility of using mosses as environmental indicators of metal pollution has been investigated. Mosses of the species Bryum argenteum were collected from different parts of Piedmont (Italy), ranging from highly polluted areas to nearly uncontaminated mountain areas. Periodical samplings were planned in every site on a monthly base, in order to check variations of metal uptake throughout one year; correlations with pluviometric and thermal patterns were investigated for all sampling stations. On every moss sample 20 elements, ranging from major (K, P, Al, Ca, Fe and Mg) to minor (Mn, Na, Ti and Zn) and trace (As, Ba, Cd, Co, Cr, Cu, Li, Ni, Pb and Sr), were quantitatively determined by inductively coupled plasma-atomic emission spectrometry or graphite furnace-atomic absorption spectrometry, depending on the needed sensitivity. Statistical analyses, carried out with principal component analysis and cluster analysis methods, revealed that a good correlation exists between metal content in mosses and pollution degree in the areas sampled.

Heat storage in alloy transformations

NASA Technical Reports Server (NTRS)

Birchenall, C. E.

1980-01-01

The feasibility of using metal alloys as thermal energy storage media was investigated. The elements selected as candidate media were limited to aluminum, copper, magnesium, silicon, zinc, calcium, and phosphorus on the basis of low cost and latent heat of transformation. Several new eutectic alloys and ternary intermetallic phases were determined. A new method employing X-ray absorption techniques was developed to determine the coefficients of thermal expansion of both the solid and liquid phases and the volume change during phase transformation. The method and apparatus are discussed and the experimental results are presented for aluminum and two aluminum-eutectic alloys. Candidate materials were evaluated to determine suitable materials for containment of the metal alloys. Graphite was used to contain the alloys during the volume change measurements. Silicon carbide was identified as a promising containment material and surface-coated iron alloys were also evaluated. System considerations that are pertinent if alloy eutectics are used as thermal energy storage media are discussed. Potential applications to solar receivers and industrial furnaces are illustrated schematically.

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

Production of aluminum-silicon alloy and ferrosilicon and commercial purity aluminum by the direct reduction process. Third interim technical report, Phase C for the period 1980 July 1-1980 September 30

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bruno, M.J.

1980-10-01

Pilot reactor VSR-3 operation in the third quarter was directed to tapping molten alloy product. Modifications to the hearth region included a tapping furnace to maintain taphole temperature, a graphite ring filter to separate carbides from matal and an alumina liner to eliminate carbiding from reaction of alloy with the graphite hearth walls. Tapping was not successful, however, due to high alloy viscosity from a large concentration of carbides. Three runs were made on the pilot crystallizer to determine the effects of alloy composition, cooling rate, tamping rate, remelt temperature and rate on eutectic Al-Si yield.

Modeling of Thermochemical Behavior in an Industrial-Scale Rotary Hearth Furnace for Metallurgical Dust Recycling

NASA Astrophysics Data System (ADS)

Wu, Yu-Liang; Jiang, Ze-Yi; Zhang, Xin-Xin; Xue, Qing-Guo; Yu, Ai-Bing; Shen, Yan-Song

2017-10-01

Metallurgical dusts can be recycled through direct reduction in rotary hearth furnaces (RHFs) via addition into carbon-based composite pellets. While iron in the dust is recycled, several heavy and alkali metal elements harmful for blast furnace operation, including Zn, Pb, K, and Na, can also be separated and then recycled. However, there is a lack of understanding on thermochemical behavior related to direct reduction in an industrial-scale RHF, especially removal behavior of Zn, Pb, K, and Na, leading to technical issues in industrial practice. In this work, an integrated model of the direct reduction process in an industrial-scale RHF is described. The integrated model includes three mathematical submodels and one physical model, specifically, a three-dimensional (3-D) CFD model of gas flow and heat transfer in an RHF chamber, a one-dimensional (1-D) CFD model of direct reduction inside a pellet, an energy/mass equilibrium model, and a reduction physical experiment using a Si-Mo furnace. The model is validated by comparing the simulation results with measurements in terms of furnace temperature, furnace pressure, and pellet indexes. The model is then used for describing in-furnace phenomena and pellet behavior in terms of heat transfer, direct reduction, and removal of a range of heavy and alkali metal elements under industrial-scale RHF conditions. The results show that the furnace temperature in the preheating section should be kept at a higher level in an industrial-scale RHF compared with that in a pilot-scale RHF. The removal rates of heavy and alkali metal elements inside the composite pellet are all faster than iron metallization, specifically in the order of Pb, Zn, K, and Na.

Development of a Standardized Approach for Assessing Potential Risks to Amphibians Exposed to Sediment and Hydric Soils

DTIC Science & Technology

2004-05-01

following digestion using method 3005A. Copper concentrations were verified using atomic absorption spectroscopy/graphite furnace. Each chamber...1995. Ammonia Variation in Sediments: Spatial, Temporal and Method -Related Effects. Environ. Toxicol. Chem. 14:1499-1506. Savage, W.K., F.W...Regulator Approved Methods and Protocols for Conducting Marine and Terrestrial Risk Assessments 1.III.01.k - Improved Field Analytical Sensors

Solidification Using a Baffle in Sealed Ampoules (SUBSA)

NASA Technical Reports Server (NTRS)

Marin, C.; Ostrogorsky, A. G.; Volz, M.; Luz, P.; Jeter, L.; Spivey, R.; Burton, H.; Smith, G.; Knowles, T. R.; Bonner, W. A.

2003-01-01

Solidification Using a Baffle in Sealed Ampoules (SUBSA) will be the first materials science experiment conducted in the Microgravity Science Glovebox (MSG) Facility at the International Space Station (ISS) Alpha. The launch is schedule for May 31, 2002. Using the specially developed furnace, 10 Te and Zn-doped single crystals of InSb will be directionally solidified in microgravity. A key goal of the SUBSA investigation is to (i) clarify the origin of the melt motion in space laboratories and (ii) to reduce the magnitude of the melt motion to the point that it does not interfere with the transport phenomena. These goals will be accomplished through a special ampoule and furnace design. A disk-shaped baffle, positioned close to the freezing front, is used to reduce melt motion. Furthermore, the solidification will be visualized by using a transparent furnace, with a video camera, continuously sending images to the earth. This allows detection of bubbles and melt de-wetting that could cause surface tension driven convection. In preparation for the space experiments, 30 ground-based experiments were conducted. The results of ground based tests and numerical modeling will be presented. Based on numerical modeling, 12 mm 1D silica ampoules were selected. The small diameter ampoule favors closer placement of the baffle to the interface, without excessive radial segregation caused by forced convection while providing more damping of natural convection. The parts in the silica ampoule include 2 carbon springs made by Energy Science Laboratories, Inc., a pyrocarbon-coated graphite cylinder, pyrocarbon-coated graphite a baffle with the shaft and the InSb charge with the seed crystal grown by W.A. Bonner of Crystallod Inc.

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.

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.

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. Copyright © 2014 Elsevier Ltd. All rights reserved.

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. Copyright © 2015 Elsevier B.V. All rights reserved.

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%.

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.

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

Qualitative and Quantitative Content Determination of Macro-Minor Elements in Bryonia Alba L. Roots using Flame Atomic Absorption Spectroscopy Technique

PubMed Central

Karpiuk, Uliana Vladimirovna; Al Azzam, Khaldun Mohammad; Abudayeh, Zead Helmi Mahmoud; Kislichenko, Viktoria; Naddaf, Ahmad; Cholak, Irina; Yemelianova, Oksana

2016-01-01

Purpose: To determine the elements in Bryonia alba L. roots, collected from the Crimean Peninsula region in Ukraine. Methods: Dry ashing was used as a flexible method and all elements were determined using atomic absorption spectrometry (AAS) equipped with flame and graphite furnace. Results: The average concentrations of the determined elements, expressed as mg/100 g dry weight of the sample, were as follow: 13.000 for Fe, 78.000 for Si, 88.000 for P, 7.800 for Al, 0.130 for Mn, 105.000 for Mg, 0.030 for Pb, 0.052 for Ni, 0.030 for Mo, 210.000 for Ca, 0.130 for Cu, 5.200 for Zn, 13.000 for Na, 1170.000 for K, 0.780 for Sr, 0.030 for Co, 0.010 for Cd, 0.010 for As, and 0.010 for Hg. Toxic elements such as Cd and Pb were also found but at very low concentration. Among the analyzed elements, K was the most abundant followed by Ca, Mg, P, Si, Fe, Na, and Zn, whereas Hg, As, Cd, Co, Mo, and Pb were found in low concentration. Conclusion: The results suggest that the roots of Bryonia alba L. plant has potential medicinal property through their high element contents present. Moreover, it showed that the AAS method is a simple, fast, and reliable for the determination of elements in plant materials. The obtained results of the current study provide justification for the usage of such fruit in daily diet for nutrition and for medicinal usage in the treatment of various diseases. PMID:27478794

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohanty, Subhasish; Majumdar, Saurindranath

Irradiation creep plays a major role in the structural integrity of the graphite components in high temperature gas cooled reactors. Finite element procedures combined with a suitable irradiation creep model can be used to simulate the time-integrated structural integrity of complex shapes, such as the reactor core graphite reflector and fuel bricks. In the present work a comparative study was undertaken to understand the effect of linear and nonlinear irradiation creep on results of finite element based stress analysis. Numerical results were generated through finite element simulations of a typical graphite reflector.

Nitrogen-doped graphene by all-solid-state ball-milling graphite with urea as a high-power lithium ion battery anode

NASA Astrophysics Data System (ADS)

Liu, Chao; Liu, Xingang; Tan, Jiang; Wang, Qingfu; Wen, Hao; Zhang, Chuhong

2017-02-01

Nitrogen-doped graphene nanosheets (NGNS) are prepared by a novel mechanochemical method via all-solid-state ball-milling graphite with urea. The ball-milling process does not only successfully exfoliate the graphite into multi-layer (<10 layers) graphene nanosheets, but at the same time, enables the N element to be doped onto the graphene. Urea, acting as a new solid doping and assist-grinding agents, has the advantages of low cost and good water solubility that can simplify the fabrication process. The as-prepared NGNS are investigated in detail by XRD, SEM, HRTEM, TGA, XPS and Raman spectroscopy. The doping nitrogens are around 3.15% and dominated (>94%) by pyrindic-N and pyrrolic-N which facilitates the NGNS with enhanced electronic conductivity and Li-ion storage capability. For the first time, we demonstrate that the all-solid-state prepared NGNS exhibits, especially at high currents, enhanced cycling stability and rate capability as Lithium ion battery (LIB) anode active material when compared to pristine graphite and undoped graphene in half-cell configuration. The method presented in this article may provide a simple, clean, economical and scalable strategy for preparation of NGNS as a feasible and promising anode material for LIBs.

A novel self-powered and sensitive label-free DNA biosensor in microbial fuel cell.

PubMed

Asghary, Maryam; Raoof, Jahan Bakhsh; Rahimnejad, Mostafa; Ojani, Reza

2016-08-15

In this work, a novel self-powered, sensitive, low-cost, and label-free DNA biosensor is reported by applying a two-chambered microbial fuel cell (MFC) as a power supply. A graphite electrode and an Au nanoparticles modified graphite electrode (AuNP/graphite electrode) were used as anode and cathode in the MFC system, respectively. The active biocatalyst in the anodic chamber was a mixed culture of microorganisms. The sensing element of the biosensor was fabricated by the well-known Au-thiol binding the ssDNA probe on the surface of an AuNP/graphite cathode. Electrons produced by microorganisms were transported from the anode to the cathode through an external circuit, which could be detected by the terminal multi-meter detector. The difference between power densities of the ssDNA probe modified cathode in the absence and presence of complementary sequence served as the detection signal of the DNA hybridization with detection limit of 3.1nM. Thereafter, this biosensor was employed for diagnosis and determination of complementary sequence in a human serum sample. The hybridization specificity studies further revealed that the developed DNA biosensor could distinguish fully complementary sequences from one-base mismatched and non-complementary sequences. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison of the morphology, chemical composition and microstructure of cryptocrystalline graphite and carbon black

NASA Astrophysics Data System (ADS)

Quan, Ying; Liu, Qinfu; Zhang, Shilong; Zhang, Shuai

2018-07-01

The structures of cryptocrystalline graphite (CG) and carbon black (CB) have been analyzed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), organic elemental analysis (OEA), X-ray diffraction (XRD), RAMAN and high-resolution transmission electron microscopy (HRTEM). These results indicate that CG has the same elemental composition as CB, with carbon being the major element present. SL sample (CG with low graphitization degree) and CB exhibit similar microcrystalline structures. CG was shown to contain a layered graphitic structure that was significantly different to the primary spherical particles present in CB. It is proposed that these CG sheets may potentially be reduced and delaminated to afford multilayer graphene structures with improved material properties.

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

PubMed

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

2012-10-01

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

MUZO flight experience with the programmable multizone furnace

NASA Technical Reports Server (NTRS)

Lockowandt, Christian; Loth, Kenneth

1993-01-01

The Multi-Zone (MUZO) furnace has been developed for growing germanium (Ge) crystals under microgravity in a Get Away Special (GAS) payload. The MUZO furnace was launched with STS-47 Endeavour in September 1992. The payload worked as planned during the flight and a Ge sample was successfully processed. The experiment has given valuable scientific information. The design and functionality of the payload together with flight experience is reported.

Oxidation Character of Carbon Composite Bricks Used in Blast Furnace

NASA Astrophysics Data System (ADS)

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

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

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

NASA Astrophysics Data System (ADS)

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

2000-12-01

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

Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

de Jesus, Alexandre; Zmozinski, Ariane Vanessa; Damin, Isabel Cristina Ferreira; Silva, Márcia Messias; Vale, Maria Goreti Rodrigues

2012-05-01

In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 μg kg- 1 for arsenic and 0.2 μg kg- 1 for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a "cold finger" was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis.

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

PubMed

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

2018-06-01

Persistent sample circulation microextraction (PSCME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was developed as a high pre-concentration technique for the determination of heavy metals in fish species. In this method, a few microliters of organic solvent (40.0 µL carbon tetrachloride) was transferred to the bottom of a conical sample cup. Then 10.0 mL of aqueous solution was transformed to fine droplets while passing through the organic solvent. At this stage, metal-ligand hydrophobic complex was extracted into the organic solvent. After extraction, 20 µL of extraction solvent was injected into the graphite tube using an auto-sampler. Under optimal conditions, enrichment factors and enhancement factor were in the range of 180-240 and 155-214, respectively. The calibration curves were linear in the range of 0.03-200 µg kg -1 and the limits of detection (LODs) were in the range of 0.01-0.05 µg kg -1 . Repeatability (intra-day) and reproducibility (inter-day) for 0.50 µg L -1 Hg and 0.10 µg L -1 Cd and Pb were in the range of 3.1-4.2% (n = 7) and 4.3-6.1% (n = 7), respectively. Potential human health risk assessment was conducted by calculating estimated weekly intake (EWI) of the metals from eating fish and comparison of these values with provisional tolerable weekly intake (PTWI) values. EWI data for the studied metals through fish consumption were lower than the PTWI values. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

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.

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

NASA Astrophysics Data System (ADS)

Chi, Se-Hwan; Kim, Gen-Chan

2008-10-01

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

CALANDRIA TYPE SODIUM GRAPHITE REACTOR

DOEpatents

Peterson, R.M.; Mahlmeister, J.E.; Vaughn, N.E.; Sanders, W.J.; Williams, A.C.

1964-02-11

A sodium graphite power reactor in which the unclad graphite moderator and fuel elements are contained within a core tank is described. The core tank is submersed in sodium within the reactor vessel. Extending longitudinally through the core thnk are process tubes with fuel elements positioned therein. A bellows sealing means allows axial expansion and construction of the tubes. Within the core tank, a leakage plenum is located below the graphite, and above the graphite is a gas space. A vent line regulates the gas pressure in the space, and another line removes sodium from the plenum. The sodium coolant flows from the lower reactor vessel through the annular space between the fuel elements and process tubes and out into the reactor vessel space above the core tank. From there, the heated coolant is drawn off through an outlet line and sent to the heat exchange. (AEC)

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. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

Reyoung Kim, Hee

2013-09-01

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

Low temperature chemical processing of graphite-clad nuclear fuels

DOEpatents

Pierce, Robert A.

2017-10-17

A reduced-temperature method for treatment of a fuel element is described. The method includes molten salt treatment of a fuel element with a nitrate salt. The nitrate salt can oxidize the outer graphite matrix of a fuel element. The method can also include reduced temperature degradation of the carbide layer of a fuel element and low temperature solubilization of the fuel in a kernel of a fuel element.

Characterization by Tin-Specific Size Exclusion Chromatography of the Free Radical Copolymerization of Tributyltin Methacrylate and Methyl Methacrylate,

DTIC Science & Technology

1980-12-11

Characterization by Tin-Specific Size Exclusion Chromatography of the Free Radical Copolymerization of Tributyltin Methacrylate and -~~~ ~~ ety Me aryate1...81 ~ 9 1 7 29 2 ABSTRACT Copolymers of tributyltin methacrylate (TBTM) and methyl methacrylate (MMA) comprise an important class of biocidal slow...exclusion chromatography (SEC); tin-specific graphite furnace atomic absorp- tion (GFAA); tributyltin methacrylate; ultraviolet absorbance; weight

Development of a certified reference material (NMIJ CRM 7505-a) for the determination of trace elements in tea leaves.

PubMed

Zhu, Yanbei; Narukawa, Tomohiro; Inagaki, Kazumi; Kuroiwa, Takayoshi; Chiba, Koichi

2011-01-01

A certified reference material (CRM) for trace elements in tea leaves has been developed in National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder (<90 µm) after frozen pulverization of washed and dried fresh tea leaves from a tea plant farm in Shizuoka Prefecture, Japan. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), high-resolution (HR-) ICP-MS, isotope-dilution (ID-) ICP-MS, inductively coupled plasma optical emission spectrometry (ICP-OES), graphite-furnace atomic-absorption spectrometry (GF-AAS) and flame atomic-absorption spectrometry (FAAS). Property values were provided for 19 elements (Ca, K, Mg, P, Al, B, Ba, Cd, Cu, Fe, Li, Mn, Na, Ni, Pb, Rb, Sr, Zn and Co) and informative values for 18 elements (Ti, V, Cr, Y, and all of the lanthanides, except for Pm whose isotopes are exclusively radioactive). The concentration ranges of property values and informative values were from 1.59% (mass) of K to 0.0139 mg kg(-1) of Cd and from 0.6 mg kg(-1) of Ti to 0.0014 mg kg(-1) of Lu, respectively. Combined relatively standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, analytical methods, characterization, calibration standard, and dry-mass correction factor. The range of the relative combined standard uncertainties was from 1.5% of Mg and K to 4.1% of Cd.

Optimization of a new methodology for trace determination of elements in biological fluids: Application for speciation of inorganic selenium in children's blood.

PubMed

Akramipour, Reza; Hemati, Mitra; Fattahi, Nazir; Pirsaheb, Meghdad; Ahmadi-Jouibari, Toraj

2017-06-05

The continuous sample drop flow microextraction (CSDFME) joined with the iridium-modified tube graphite furnace atomic absorption spectrometry (GFAAS) has been developed as a highly sensitive technique for the speciation of selenium in blood samples. In this method 32.0μl carbon tetrachloride is transferred to the bottom of a conical sample cup. Then the 5.0ml of aqueous solution transforms to fine droplets while passing through the organic solvent. At this stage, Se(IV)-APDC hydrophobic complex is extracted into the organic solvent. After extraction, the conical sample cup is transferred to the GFAAS and 20μl of extraction solvent was injected into the graphite tube by the aim of autosampler. Under the optimum conditions, the calibration graph was linear in the range of 0.06-3.0μgl -1 with detection limit of 0.02μgl -1 . The enrichment factor and enhancement factor were 106 and 91, respectively. Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 2.5μgl -1 of selenium were 3.7% and 4.2%, respectively. Total inorganic Se(IV, VΙ) was measured after reduction of Se(VΙ) with gentle boiling in 5M HCl medium for 50min and adjusting pH to 3, and the concentration of Se(VΙ) was calculated by subtracting the Se(IV) concentration from the total selenium concentration. Copyright © 2017 Elsevier B.V. All rights reserved.

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

USGS Publications Warehouse

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

1984-01-01

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

Cadmium contamination in cereal-based diets and diet ingredients

DOE Office of Scientific and Technical Information (OSTI.GOV)

Siitonen, P.H.; Thompson, H.C. Jr.

1990-11-01

Cereal-based diet and/or diet ingredient cadmium levels were determined by graphite furnace AAS. Cadmium contamination was 88.3 and 447 ppb in two cereal-based diets, 44.6 and 48.9 ppb in two purified diets, and ranged from less than 1.1 to 22,900 ppb in the ingredients of one cereal-based diet. The major source of cadmium contamination was attributed to the calcium supplement used for diet formulation. Comparative analyses of two purified diet samples and one cereal-based diet by the National Institute of Standards and Technology (NIST, formerly the National Bureau of Standards) and the National Center for Toxicological Research (NCTR) gave virtuallymore » identical results for Cd. A comparative study of Cd levels determined by flame and furnace AAS was also made by the NCTR and the NIST.« less

Graphite-based photovoltaic cells

DOEpatents

Lagally, Max; Liu, Feng

2010-12-28

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

Multielement extraction system for determining 19 trace elements in gold exploration samples

USGS Publications Warehouse

Clark, J. Robert; Viets, John G.; ,

1990-01-01

A multielement extraction system is being used successfully to provide essentially interference-free geochemical analyses to aid in gold exploration. The Methyl isobutyl ketone-Amine synerGistic Iodide Complex (MAGIC) extraction system separates Ag, As, Au, Bi, Cd, Cu, Ga, Hg, In, Mo, Pb, Pd, Pt, Sb, Se, Sn, Te, Tl, and Zn from interfering geological matrices. Quantitative extraction of these elements is accomplished over a broad range of acid normality making it possible to economically determine all 19 elements from a single digestion or leach solution. The resulting organic extracts are amenable to analysis by inductively coupled plasma atomic emission spectroscopy (ICP-AES) and flame atomic absorption spectroscopy (FAAS). For many years the principal shortcoming of ICP-AES was the complex spectral and stray-light interferences that were caused by the extreme variability of components such as Fe, Na, and Ca in common geological matrices. The MAGIC extraction allows determination of the extracted elements with enhanced sensitivity, from a virtually uniform matrix, by ICP-AES and FAAS. Because of its simultaneous multichannel capabilities, ICP-AES is the ideal instrumental technique for determining these 19 extracted elements. Ultratrace (sub-part-per-billion) determinations of Au and many of the other extracted elements can be made by graphite furnace atomic absorption spectroscopy (GFAAS), following back stripping of the extracts. The combination of the extraction followed by stripping of the organic phase eliminates 99.999% of potential interferences for Au. Gold determination by GFAAS from these extracts under the specified conditions yields a fourfold improvement in sensitivity over conventional GFAAS methods. This sensitivity enhancement and the interference-free matrix allow highly reliable determinations well into the parts-per-trillion range.

NUCLEAR REACTOR ELEMENT

DOEpatents

Sanz, M.C.; Scully, C.N.

1961-06-27

The patented fuel element is a hexagonal graphite body having an axial channel therethrough. The graphite is impregnated with uranium which is concentrated near the axial channel. Layers of tantalum nitride and tantalum carbide are disposed on the surface of the body confronting the channel.

Synthesis of Multi-Walled Carbon Nanotubes from Plastic Waste Using a Stainless-Steel CVD Reactor as Catalyst.

PubMed

Tripathi, Pranav K; Durbach, Shane; Coville, Neil J

2017-09-22

The disposal of non-biodegradable plastic waste without further upgrading/downgrading is not environmentally acceptable and many methods to overcome the problem have been proposed. Herein we indicate a simple method to make high-value nanomaterials from plastic waste as a partial solution to the environmental problem. Laboratory-based waste centrifuge tubes made of polypropylene were chosen as a carbon source to show the process principle. In the process, multi-walled carbon nanotubes (MWCNTs) were synthesized from plastic waste in a two-stage stainless steel 316 (SS 316) metal tube that acted as both reactor vessel and catalyst. The steel reactor contains Fe (and Ni, and various alloys), which act as the catalyst for the carbon conversion process. The reaction and products were studied using electron probe microanalysis, thermogravimetric analysis, Raman spectroscopy and transmission electron microscopy and scanning electron microscopy. Optimization studies to determine the effect of different parameters on the process showed that the highest yield and most graphitized MWCNTs were formed at 900 °C under the reaction conditions used (yield 42%; Raman I D / I G ratio = 0.48). The high quality and high yield of the MWCNTs that were produced in a flow reactor from plastic waste using a two stage SS 316 chemical vapor deposition (CVD) furnace did not require the use of an added catalyst.

Synthesis of Multi-Walled Carbon Nanotubes from Plastic Waste Using a Stainless-Steel CVD Reactor as Catalyst

PubMed Central

Durbach, Shane

2017-01-01

The disposal of non-biodegradable plastic waste without further upgrading/downgrading is not environmentally acceptable and many methods to overcome the problem have been proposed. Herein we indicate a simple method to make high-value nanomaterials from plastic waste as a partial solution to the environmental problem. Laboratory-based waste centrifuge tubes made of polypropylene were chosen as a carbon source to show the process principle. In the process, multi-walled carbon nanotubes (MWCNTs) were synthesized from plastic waste in a two-stage stainless steel 316 (SS 316) metal tube that acted as both reactor vessel and catalyst. The steel reactor contains Fe (and Ni, and various alloys), which act as the catalyst for the carbon conversion process. The reaction and products were studied using electron probe microanalysis, thermogravimetric analysis, Raman spectroscopy and transmission electron microscopy and scanning electron microscopy. Optimization studies to determine the effect of different parameters on the process showed that the highest yield and most graphitized MWCNTs were formed at 900 °C under the reaction conditions used (yield 42%; Raman ID/IG ratio = 0.48). The high quality and high yield of the MWCNTs that were produced in a flow reactor from plastic waste using a two stage SS 316 chemical vapor deposition (CVD) furnace did not require the use of an added catalyst. PMID:28937596

GFAAS determination of selenium in infant formulas using a microwave digestion method.

PubMed

Alegria, A; Barbera, R; Farré, R; Moreno, A

1994-01-01

A method for determining the selenium content of infant formulas is proposed. It includes wet digestion with nitric acid and hydrogen peroxide in medium pressure teflon bombs in a microwave oven and determination by graphite furnace atomic absorption spectrometry (GFAAS). The absence of interferences is checked. Values obtained for the limit of detection (19.4 ng/g), precision (RSD = 2.2%) and accuracy by analysis of a reference material show that the method is reliable.

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.

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.

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. Copyright © 2016 Elsevier B.V. All rights reserved.

Production of fullerenes with concentrated solar flux

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hale, M. J.; Fields, C.; Lewandowski, A.

1994-01-01

Research at the National Renewable Energy Laboratory (NREL) has demonstrated that fullerenes can be produced using highly concentrated sunlight from a solar furnace. Since they were first synthesized in 1989, fullerenes have been the subject of intense research. They show considerable commercial potential in advanced materials and have potential applications that include semiconductors, superconductors, high-performance metals, and medical technologies. The most common fullerene is C{sub 60}, which is a molecule with a geometry resembling a soccer ball. Graphite vaporization methods such as pulsed-laser vaporization, resistive heating, and carbon arc have been used to produce fullerenes. None of these, however, seemsmore » capable of producing fullerenes economically on a large scale. The use of concentrated sunlight may help avoid the scale-up limitations inherent in more established production processes. Recently, researchers at NREL made fullerenes in NREL`s 10 kW High Flux Solar Furnace (HFSF) with a vacuum reaction chamber designed to deliver a solar flux of 1200 W/cm{sup 2} to a graphite pellet. Analysis of the resulting carbon soot by mass spectrometry and high-pressure liquid chromatography confirmed the existence of fullerenes. These results are very encouraging and we are optimistic that concentrated solar flux can provide a means for large-scale, economical production of fullerenes. This paper presents our method, experimental apparatus, and results of fullerene production research performed with the HFSF.« less

Determination of dietary cadmium-induced metallothioneins in rabbit kidneys and cadmium in metallothioneins by anion-exchange high-performance liquid chromatography coupled with graphite furnace atomic absorption spectrometry.

PubMed

Peng, S; Shan, X Q; Zheng, Y; Jin, L Z; Xu, W B

1991-12-06

A rapid method is described for the determination of dietary cadmium-induced metallothioneins (MTs) in rabbit kidneys by anion-exchange high-performance liquid chromatography. Rabbit kidney MT-I and MT-II were eluted at ca. 15.0 and 18.8 min, respectively, from a DEAE-5PW anion-exchange column with a Tris-HCl buffer (0.01-0.25 M, pH 8.6) and detected by ultraviolet absorbance at 254 nm. A standard calibration curve was constructed using purified standard MT isoforms, which demonstrated an excellent linear correlation between UV absorbance peak heights and the amounts of MT isoforms. Feeding a dose of cadmium for some days resulted in an increase in MT concentrations in rabbit kidneys, but not in the livers. The cadmium concentrations in MT-I and MT-II elutions were determined by graphite furnace atomic absorption spectrometry. MT-I and MT-II showed some differences associated with the oral intake of cadmium. Dietary cadmium also caused zinc to accumulate in kidneys to some extent. The effects of dietary oleic acid on the synthesis of MTs were also studied. Based on the method of standard additions, the recovery of MTs exceeded 93% and replicated injection of samples yielded a relative standard deviation of 2.4% at an MT level of 280 micrograms/g.

Ultra-high vacuum compatible preparation chain for intermetallic compounds

NASA Astrophysics Data System (ADS)

Bauer, A.; Benka, G.; Regnat, A.; Franz, C.; Pfleiderer, C.

2016-11-01

We report the development of a versatile material preparation chain for intermetallic compounds, which focuses on the realization of a high-purity growth environment. The preparation chain comprises an argon glovebox, an inductively heated horizontal cold boat furnace, an arc melting furnace, an inductively heated rod casting furnace, an optically heated floating-zone furnace, a resistively heated annealing furnace, and an inductively heated annealing furnace. The cold boat furnace and the arc melting furnace may be loaded from the glovebox by means of a load-lock permitting to synthesize compounds starting with air-sensitive elements while handling the constituents exclusively in an inert gas atmosphere. All furnaces are all-metal sealed, bakeable, and may be pumped to ultra-high vacuum. We find that the latter represents an important prerequisite for handling compounds with high vapor pressure under high-purity argon atmosphere. We illustrate the operational aspects of the preparation chain in terms of the single-crystal growth of the heavy-fermion compound CeNi2Ge2.

Improvement of calculation method for electrical parameters of short network of ore-thermal furnaces

NASA Astrophysics Data System (ADS)

Aliferov, A. I.; Bikeev, R. A.; Goreva, L. P.

2017-10-01

The paper describes a new calculation method for active and inductive resistance of split interleaved current leads packages in ore-thermal electric furnaces. The method is developed on basis of regression analysis of dependencies of active and inductive resistances of the packages on their geometrical parameters, mutual disposition and interleaving pattern. These multi-parametric calculations have been performed with ANSYS software. The proposed method allows solving split current lead electrical parameters minimization and balancing problems for ore-thermal furnaces.

Multi-Scale Modeling of a Graphite-Epoxy-Nanotube System

NASA Technical Reports Server (NTRS)

Frankland, S. J. V.; Riddick, J. C.; Gates, T. S.

2005-01-01

A multi-scale method is utilized to determine some of the constitutive properties of a three component graphite-epoxy-nanotube system. This system is of interest because carbon nanotubes have been proposed as stiffening and toughening agents in the interlaminar regions of carbon fiber/epoxy laminates. The multi-scale method uses molecular dynamics simulation and equivalent-continuum modeling to compute three of the elastic constants of the graphite-epoxy-nanotube system: C11, C22, and C33. The 1-direction is along the nanotube axis, and the graphene sheets lie in the 1-2 plane. It was found that the C11 is only 4% larger than the C22. The nanotube therefore does have a small, but positive effect on the constitutive properties in the interlaminar region.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ganesh, Panchapakesan; Kent, Paul R; Mochalin, Vadym N

We simulate the experimentally observed graphitization of nanodiamonds into multi-shell onion-like carbon nanostructures, also called carbon onions, at different temperatures, using reactive force fields. The simulations include long-range Coulomb and van der Waals interactions. Our results suggest that long-range interactions play a crucial role in the phase-stability and the graphitization process. Graphitization is both enthalpically and entropically driven and can hence be controlled with temperature. The outer layers of the nanodiamond have a lower kinetic barrier toward graphitization irrespective of the size of the nanodiamond and graphitize within a few-hundred picoseconds, with a large volume increase. The inner core ofmore » the nanodiamonds displays a large size-dependent kinetic barrier, and graphitizes much more slowly with abrupt jumps in the internal energy. It eventually graphitizes by releasing pressure and expands once the outer shells have graphitized. The degree of transformation at a particular temperature is thereby determined by a delicate balance between the thermal energy, long-range interactions, and the entropic/enthalpic free energy gained by graphitization. Upon full graphitization, a multi-shell carbon nanostructure appears, with a shell-shell spacing of about {approx}3.4 {angstrom} for all sizes. The shells are highly defective with predominantly five- and seven-membered rings to curve space. Larger nanodiamonds with a diameter of 4 nm can graphitize into spiral structures with a large ({approx}29-atom carbon ring) pore opening on the outermost shell. Such a large one-way channel is most attractive for a controlled insertion of molecules/ions such as Li ions, water, or ionic liquids, for increased electrochemical capacitor or battery electrode applications.« less

Furnace Cyclic Oxidation Behavior of Multi-Component Low Conductivity Thermal Barrier Coatings

NASA Technical Reports Server (NTRS)

Zhu, Dong-Ming; Nesbitt, James A.; Barrett, Charles A.; McCue, Terry R.; Miller, Robert A.

2004-01-01

Ceramic thermal barrier coatings will play an increasingly important role in advanced gas turbine engines because of their ability to further increase engine operating temperatures and reduce cooling, thus helping achieve future engine low emission, high efficiency and improved reliability goals. Advanced multi-component zirconia-based thermal barrier coatings are being developed using an oxide defect clustering design approach to achieve the required coating low thermal conductivity and high temperature stability. Although the new composition coatings were not yet optimized for cyclic durability, an initial durability screening of the candidate coating materials was conducted using conventional furnace cyclic oxidation tests. In this paper, furnace cyclic oxidation behavior of plasma-sprayed zirconia-based defect cluster thermal barrier coatings was investigated at 1163 C using 45 min hot cycles. The ceramic coating failure mechanisms were studied using scanning electron microscopy (SEM) combined with X-ray diffraction (XRD) phase analysis after the furnace tests. The coating cyclic lifetime is also discussed in relation to coating processing, phase structures, dopant concentration, and other thermo-physical properties.

RECOVERY OF VALUABLE MATERIAL FROM GRAPHITE BODIES

DOEpatents

Fromm, L.W. Jr.

1959-09-01

An electrolytic process for recovering uranium from a graphite fuel element is described. The uraniumcontaining graphite body is disposed as the anode of a cell containing a nitric acid electrolyte and a 5 amp/cm/sup 2/ current passed to induce a progressive disintegration of the graphite body. The dissolved uranium is quickly and easily separated from the resulting graphite particles by simple mechanical means, such as centrifugation, filtration, and decontamination.

Trace elements and heavy metals in mineral and bottled drinking waters on the Iranian market.

PubMed

Hadiani, Mohammad Rasoul; Dezfooli-Manesh, Shirin; Shoeibi, Shahram; Ziarati, Parisa; Mousavi Khaneghah, Amin

2015-01-01

A survey of Iranian waters, sampled from 2010 to 2013, is presented. A total of 128 water samples from 42 different brands of bottled mineral and drinking water were collected and analysed for contamination levels of lead (Pb), cadmium (Cd), copper (Cu), arsenic (As) and mercury (Hg). Determinations were performed using a graphite furnace atomic absorption spectrophotometer for Pb, Cd and Cu, a hydride vapour generation as well as an Arsenator digital kit (Wagtech WTD, Tyne and Wear, UK) for As and a direct mercury analyser for Hg. Arsenic concentration in six bottled gaseous mineral samples was higher than the related limit. Regardless of these, mean concentrations of Pb, Cd, Cu, As and Hg in all types of water samples were 4.50 ± 0.49, 1.08 ± 0.09, 16.11 ± 2.77, 5.80 ± 1.63 and 0.52 ± 0.03 µg L⁻¹, respectively. Values obtained for analysed heavy metals in all samples were permissible according to the limits of national and international standards.

The biocorrosion of copper by biopolymers as examined in situ, in real time FT-IR/CIR/ATR in conjunction with pre and post XPS/AES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gianotto, A.K.; Wichlacz, P.L.; Jolley, J.G.

1989-01-01

Thin films of copper (2.0 nm on germanium internal reflection elements (IREs) and 3.4 nm on germanium discs) were exposed to 10% gum arabic (aqueous solution), 2% alginic acid (aqueous solution), 1% bacterial culture supernatant (BCS, simulated seawater solution) and 0.5% Pseudomonas atlantica exopolymer (simulated seawater solution). The IREs were monitored in situ, in real time using fourier transform infrared/cylindrical internal reflection/attenuated total reflection spectroscopy as a function of time at ambient conditions. The discs were characterized (pre- and post-exposure) by x-ray photoelectron and Auger electron spectroscopies. Ancillary graphite furnace atomic absorption spectroscopy was used to monitor the removal processmore » of the copper thin film from the germanium substrates. Results indicate that Cu was oxidized by gum arabic, alginic acid and BCS. Furthermore, Cu was removed from the Cu/Ge interface by all four polymers. The Cu was found associated with the polymer solutions. 20 refs., 6 figs., 1 tab.« less

The influence of industrial-scale canning on cadmium and lead levels in sardines and anchovies from commercial fishing centres of the Mediterranean Sea.

PubMed

Galitsopoulou, Augoustina; Georgantelis, Dimitrios; Kontominas, Michael

2012-01-01

The current study encompassed a survey on the levels of toxic trace elements in two highly consumed fish species in commercial fishing centres of western, central and eastern Mediterranean Sea. A Zeeman GTA-AAS graphite furnace atomic absorption spectrometry system was used throughout the study. Toxicological evaluation of the samples revealed a low Cd content in the raw samples, ranging between 0.003 and 0.027 mg kg⁻¹. Pb presented significantly higher values, from 0.037 to 0.297 mg kg⁻¹, occasionally reaching the limit of 0.3 mg kg⁻¹. Heavy metal levels were particularly higher in bones, thus raising queries about the safe consumption of fish intended to be eaten as a whole, a very common practice for small fish and canned products. The influence of industrial-scale canning showed that canning enhanced heavy metal levels by 35%-80%. The effect of canning depended on metal type and reduction of moisture loss after the steam-roasting step of the canning procedure.

Ambient concentrations of total suspended particulate matter and its elemental constituents at the wider area of the mining facilities of TVX Hellas in Chalkidiki, Greece.

PubMed

Gaidajis, George

2003-01-01

To assess ambient air quality at the wider area of TVX Hellas mining facilities, the Total Suspended Particulate matter (TSP) and its content in characteristic elements, i.e., As, Cd, Cu, Fe, Mn, Pb, Zn are being monitored for more than thirty months as part of the established Environmental Monitoring Program. High Volume air samplers equipped with Tissue Quartz filters were employed for the collection of TSP. Analyses were effected after digestion of the suspended particulate with an HNO3-HCl solution and determination of elemental concentrations with an Atomic Absorption Spectroscopy equipped with graphite furnace. The sampling stations were selected to record representatively the existing ambient air quality in the vicinity of the facilities and at remote sites not affected from industrial activities. Monitoring data indicated that the background TSP concentrations ranged from 5-60 microg/m3. Recorded TSP concentrations at the residential sites close to the facilities ranged between 20-100 microg/m3, indicating only a minimal influence from the mining and milling activities. Similar spatial variation was observed for the TSP constituents and specifically for Pb and Zn. To validate the monitoring procedures, a parallel sampling campaign took place with different High Volume samplers at days where low TSP concentrations were expected. The satisfactory agreement (+/- 11%) at low concentrations (50-100 microg/m3) clearly supported the reproducibility of the techniques employed specifically at the critical range of lower concentrations.

Zircon Carburation Studies as Intermediate Stage in the Zirconium Fabrication; ESTUDIOS ENCAMINADOS A LA CARBURACTION DEL CIRON COMO ETAPA INTERMEDIA EN LA OBTENCION DE CIRCONIO

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huertas, V.A.; Gonzalez, L.S.; Lopez, M.

1963-01-01

Zirconium carbide and carbonitride mixtures were obtained by Kroll's method. Reaction products were identified by micrography and x-ray diffraction analysis. The optimum graphite content in the initial charge for the carburization reaction was studied. Zirconium, silicon, and carbon content in the final product was controlled as a function of current in the furnace and reaction time. Further chlorination of the final product was performed successfully. (auth)

Morphological Characterization Of Titania Slag Obtained From Red Sediment Placer Ilmenite Using Microwave Energy

NASA Astrophysics Data System (ADS)

Srikant, S. S.; Mukherjee, P. S.; Bhima Rao, R.

2015-04-01

This paper deals with the main objective to observe the effect of microwave heat treatment for the production of Titania rich slag and pig iron from placer ilmenite. The experiments carried out in the present investigation on the oxidized ilmenite sample for microwave heat treatment in microwave sintering furnace reveals that a product can be obtained containing Titania rich slag and metalized iron. The in-depth characterisation of these products using SEM-EDAX shows that around 75-85 % of titanium dioxide is formed in terms of titania rich slag by using microwave sintering furnace after reduction of oxidized ilmenite with proper stoichiometric graphitic carbon and silicon carbide (SiC) susceptor. The titania rich slag is considered to be better input material for production of pigment grade titanium dioxide. On the other hand, the pig iron obtained as by product from titania rich slag is also important for automobile and steel industries application.

Elemental Zinc Is Inversely Associated with C-Reactive Protein and Oxidative Stress in Chronic Liver Disease.

PubMed

Uddin, Md Giash; Hossain, Mohammad Salim; Rahman, Md Atiqur; Uddin, A H M Mazbah; Bhuiyan, Md Shafiullah

2017-08-01

Chronic liver disease (CLD) is associated with the destruction of liver parenchyma cell. It is the main cause of morbidity and mortality in most of the developed countries. Oxidative stress and altered levels of different trace elements in serum have been documented for different diseases including inflammation and many liver diseases. This study aims to evaluate the serum level of malondialdehyde (MDA), nitric oxide (NO), antioxidant vitamin C, C-reactive protein (CRP), and zinc (Zn) in CLD patients and to establish a correlation among the study parameters with the severity of inflammatory conditions of CLD. In this study, CLD patients and healthy volunteers were recruited. Total cholesterol and triglyceride were determined by colorimeter using enzymatic method. Serum non-enzymatic antioxidant vitamin C, reactive oxygen species nitric oxide (NO), and malondialdehyde (MDA) were determined by UV-spectrophotometric method. Trace element (Zn) levels were determined by graphite furnace atomic absorption spectroscopy. Independent sample t test and Pearson's correlation test were performed for statistical analysis using the statistical software package SPSS, Version 20. Studies showed that the MDA (p < 0.001), NO (p < 0.001), and CRP levels were significantly higher in CLD patients than in control subjects. The antioxidant vitamin C (p < 0.001) and trace element zinc (p < 0.001) were comparatively lower in the CLD patients than in control subjects. Elemental Zn showed an inverse relationship with MDA, NO, and CRP but positively correlated with antioxidant capacity, whereas MDA showed a positive correlation with CRP level. Thus, we conclude that attenuated level of Zn and antioxidant in serum play an important role in the inflammatory status of CLD patients by elevating the concentration of MDA, NO, and CRP.

Minimally-invasive Laser Ablation Inductively Coupled Plasma Mass Spectrometry analysis of model ancient copper alloys

NASA Astrophysics Data System (ADS)

Walaszek, Damian; Senn, Marianne; Wichser, Adrian; Faller, Markus; Wagner, Barbara; Bulska, Ewa; Ulrich, Andrea

2014-09-01

This work describes an evaluation of a strategy for multi-elemental analysis of typical ancient bronzes (copper, lead bronze and tin bronze) by means of laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS).The samples originating from archeological experiments on ancient metal smelting processes using direct reduction in a ‘bloomery’ furnace as well as historical casting techniques were investigated with the use of the previously proposed analytical procedure, including metallurgical observation and preliminary visual estimation of the homogeneity of the samples. The results of LA-ICPMS analysis were compared to the results of bulk composition obtained by X-ray fluorescence spectrometry (XRF) and by inductively coupled plasma mass spectrometry (ICPMS) after acid digestion. These results were coherent for most of the elements confirming the usefulness of the proposed analytical procedure, however the reliability of the quantitative information about the content of the most heterogeneously distributed elements was also discussed in more detail.

Design and Development of an Acoustic Levitation System for Use in CVD Growth of Carbon Nanotubes

NASA Astrophysics Data System (ADS)

Qasem, Amal ali

The most widely used methods for growth of carbon nanotubes (CNTs) arc discharge, laser ablation, and chemical vapor deposition (CVD). Some of these methods have difficulties, such as controlling the quality and straightness of the nanotube in the synthesis of CNTs from substrates. Also, the enhanced plasma chemical vapor deposition method with the catalyst on a substrate produces straighter, larger diameter nanotubes by the tip growth method, but they are short. The difficulty in the floating catalyst method is that the nanotubes stay in the growth furnace for short times limiting growth to about one mm length; this method also leaves many catalyst impurities. One factor that limits CNT growth in these methods is the difficulty of getting enough carbon atoms to the growth catalyst to grow long nanotubes. The motivation of this work is that longer, higher quality nanotubes could be grown by increasing growth time and by increasing carbon atom movement to catalyst. The goal of this project is to use acoustic levitation to assist chemical vapor deposition growth by trapping and vibrating the growing CNTs for better properties. Our levitation system consists of a piezoelectric transducer attached to an aluminum horn and quartz rod extending into the growth furnace. The most important elements of our methods to achieve the acoustic levitation are as follows. 1. Using COMSOL Multi-physic Simulation software to determine the length of quartz rod needed to excite standing waves for levitation in the tube furnace. 2. Determining the resonance frequency of different transducers and horns. 3. Using ultrasound measurement to determine the time of flight, velocity of sound and sound wavelength of different horns. 4. Making Aluminum horns with the appropriate lengths. 5. Using ultrasound measurement to determine the changing of quartz rod velocity of sound and length in the furnace. 6. Mounting the transducer to booster horn and aluminum cylindrical horn above a reflector to produce the standing waves. The levitation of small Styrofoam balls was successful by using this system and verified wavelengths of standing wave and position of levitation. We could not levitate powders, most likely due to electrostatic charging, air currents, but most importantly insufficient power to drive transducer. In addition, we built a CVD growth furnace with ultrasound transducer- horn- quartz rod and reflector. The reflector support also included a sense piezoelectric element for determining standing wave strength. This reflector support was mounted on a linear translation stage to control the quartz rod-reflector separation to produce standing waves. To remove the contaminated unwanted CNTs, we built a separate tube furnace tube filled with a molecular sieve to burn the CNT's in air. Finally, we made catalyst-coated, ceramic microparticles for levitation and used these to verify CNT growth. Future efforts research would be to levitate these micro particles at room temperature then in the high temperature furnace for growth of carbon nanotubes.

Studies on the Processing Methods for Extraterrestrial Materials

NASA Technical Reports Server (NTRS)

Grimley, R. T.; Lipschutz, M. E.

1984-01-01

The literature was surveyed for high temperature mass spectrometric research on single oxides, complex oxides, and minerals in an effort to develop a means of separating elements and compounds from lunar and other extraterrestrial materials. A data acquisition system for determining vaporization rates as a function of time and temperature and software for the IEEE-488 Apple-ORTEC interface are discussed. Experimental design information from a 1000 C furnace were used with heat transfer calculations to develop the basic design for a 1600 C furnace. A controller was built for the higher temperature furnace and drawings are being made for the furnace.

Identification and control of a multizone crystal growth furnace

NASA Technical Reports Server (NTRS)

Batur, C.; Sharpless, R. B.; Duval, W. M. B.; Rosenthal, B. N.; Singh, N. B.

1992-01-01

This paper presents an intelligent adaptive control system for the control of a solid-liquid interface of a crystal while it is growing via directional solidification inside a multizone transparent furnace. The task of the process controller is to establish a user-specified axial temperature profile and to maintain a desirable interface shape. Both single-input-single-output and multi-input-multi-output adaptive pole placement algorithms have been used to control the temperature. Also described is an intelligent measurement system to assess the shape of the crystal while it is growing. A color video imaging system observes the crystal in real time and determines the position and the shape of the interface. This information is used to evaluate the crystal growth rate, and to analyze the effects of translational velocity and temperature profiles on the shape of the interface. Creation of this knowledge base is the first step to incorporate image processing into furnace control.

Crewmember working on the spacelab Zeolite Crystal Growth experiment.

NASA Technical Reports Server (NTRS)

1992-01-01

View showing Payload Specialists Bonnie Dunbar and Larry DeLucas in the aft section of the U. S. Microgravity Laboratory-1. Dunbar is preparing to load a sample in the Crystal Growth Furnace (CGF) Integrated Furnace Experiment Assembly (IFEA) in rack 9 of the Microgravity Laboratory. DeLucas is checking out the multi-purpose Glovebox Facility.

Formation, characterization, and dynamics of onion-like carbon structures for electrical energy storage from nanodiamonds using reactive force fields

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ganesh, P.; Kent, P. R. C.; Mochalin, V.

We simulate the experimentally observed graphitization of nanodiamonds into multi-shell onion-like carbonnanostructures, also called carbon onions, at different temperatures, using reactive force fields. The simulations include long-range Coulomb and van der Waals interactions. Our results suggest that long-range interactions play a crucial role in the phase-stability and the graphitization process. Graphitization is both enthalpically and entropically driven and can hence be controlled with temperature. The outer layers of the nanodiamond have a lower kinetic barrier toward graphitization irrespective of the size of the nanodiamond and graphitize within a few-hundred picoseconds, with a large volume increase. The inner core of themore » nanodiamonds displays a large size-dependent kinetic barrier, and graphitizes much more slowly with abrupt jumps in the internal energy. It eventually graphitizes by releasing pressure and expands once the outer shells have graphitized. The degree of transformation at a particular temperature is thereby determined by a delicate balance between the thermal energy, long-range interactions, and the entropic/enthalpic free energy gained by graphitization. Upon full graphitization, a multi-shell carbonnanostructure appears, with a shell-shell spacing of about ~3.4 Å for all sizes. The shells are highly defective with predominantly five- and seven-membered rings to curve space. Larger nanodiamonds with a diameter of 4 nm can graphitize into spiral structures with a large (~29-atom carbon ring) pore opening on the outermost shell. Such a large one-way channel is most attractive for a controlled insertion of molecules/ions such as Li ions, water, or ionic liquids, for increased electrochemical capacitor or battery electrode applications.« less

Formation, characterization and dynamics of onion like carbon structures from nanodiamonds using reactive force-fields for electrical energy storage

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kent, Paul R

We simulate the experimentally observed graphitization of nanodiamonds into multi-shell onion-like carbon nanostructures, also called carbon onions, at different temperatures, using reactive force fields. The simulations include long-range Coulomb and van der Waals interactions. Our results suggest that long-range interactions play a crucial role in the phase-stability and the graphitization process. Graphitization is both enthalpically and entropically driven and can hence be controlled with temperature. The outer layers of the nanodiamond have a lower kinetic barrier toward graphitization irrespective of the size of the nanodiamond and graphitize within a few-hundred picoseconds, with a large volume increase. The inner core ofmore » the nanodiamonds displays a large size-dependent kinetic barrier, and graphitizes much more slowly with abrupt jumps in the internal energy. It eventually graphitizes by releasing pressure and expands once the outer shells have graphitized. The degree of transformation at a particular temperature is thereby determined by a delicate balance between the thermal energy, long-range interactions, and the entropic/enthalpic free energy gained by graphitization. Upon full graphitization, a multi-shell carbon nanostructure appears, with a shell-shell spacing of about {approx}3.4 {angstrom} for all sizes. The shells are highly defective with predominantly five- and seven-membered rings to curve space. Larger nanodiamonds with a diameter of 4 nm can graphitize into spiral structures with a large ({approx}29-atom carbon ring) pore opening on the outermost shell. Such a large one-way channel is most attractive for a controlled insertion of molecules/ions such as Li ions, water, or ionic liquids, for increased electrochemical capacitor or battery electrode applications.« less

Microgravity

NASA Image and Video Library

1995-09-15

Large Isothermal Furnace (LIF) was flown on a mission in cooperation with the National Space Development Agency (NASDA) of Japan. LIF is a vacuum-heating furnace designed to heat large samples uniformly. The furnace consists of a sample container and heating element surrounded by a vacuum chamber. A crewmemeber will insert a sample cartridge into the furnace. The furnace will be activated and operations will be controlled automatically by a computer in response to an experiment number entered on the control panel. At the end of operations, helium will be discharged into the furnace, allowing cooling to start. Cooling will occur through the use of a water jacket while rapid cooling of samples can be accomplished through a controlled flow of helium. Data from experiments will help scientists better understand this important process which is vital to the production of high-quality semiconductor crystals.

On diamond, graphitic and amorphous carbons in primitive extraterrestrial solar system materials

NASA Technical Reports Server (NTRS)

Rietmeijer, Frans J. M.

1990-01-01

Carbon is among the most abundant elements in the universe and carbon chemistry in meteorites and comets is an important key to understanding many Solar System and interstellar processes. Yet, the mineralogical properties and interrelations between various structural forms of elemental carbon remain ambiguous. Crystalline elemental carbons include rhombohedral graphite, hexagonal graphite, cubic diamond, hexagonal diamond (i.e., lonsdaleite or carbon-2H) and chaoite. Elemental carbon also occurs as amorphous carbon and poorly graphitized (or turbostratic) carbon but of all the forms of elemental carbon only graphite is stable under physical conditions that prevail in small Solar System bodies and in the interstellar medium. The recent discovery of cubic diamond in carbonaceous chondrites and hexagonal diamond in chondritic interplanetary dust particles (IDPs) have created a renewed interest in the crystalline elemental carbons that were not formed by shock processes on a parent body. Another technique, Raman spectroscopy, confirms a widespread occurrence of disordered graphite in the Allende carbonaceous chondrite and in chondritic IDPs. Elemental carbons have also been identified by their characteristic K-edge features in electron energy loss spectra (EELS). However, the spectroscopic data do not necessarily coincide with those obtained by selected area electron diffraction (SAED). In order to interpret these data in terms of rational crystalline structures, it may be useful to consider the principles underlying electron diffraction and spectroscopic analyses. Electron diffraction depends on electron scattering, on the type of atom and the distance between atoms in a crystal lattice. Spectroscopic data are a function of the type of atom and the energy of bonds between atoms. Also, SAED is a bulk sampling technique when compared to techniques such as Raman spectroscopy or EELS. Thus, it appears that combined analyses provide contradictory results and that amorphous, or short-range ordered, carbon identified by conventional TEM imaging and SAED may show evidence for sp(3) bonds in EELS spectra. It is suggested that complex, nanometer-scale, mineralogical interrelations are common to all elemental carbons irrespective of their origin. The subsequent thermal history, or energy balance, will determine the ultimate microstructure.

Oil Palm Waste-Based Precursors as a Renewable and Economical Carbon Sources for the Preparation of Reduced Graphene Oxide from Graphene Oxide

PubMed Central

Nasir, Salisu; Hussein, Mohd Zobir; Yusof, Nor Azah; Zainal, Zulkarnain

2017-01-01

Herein, a new approach was proposed to produce reduced graphene oxide (rGO) from graphene oxide (GO) using various oil palm wastes: oil palm leaves (OPL), palm kernel shells (PKS) and empty fruit bunches (EFB). The effect of heating temperature on the formation of graphitic carbon and the yield was examined prior to the GO and rGO synthesis. Carbonization of the starting materials was conducted in a furnace under nitrogen gas for 3 h at temperatures ranging from 400 to 900 °C and a constant heating rate of 10 °C/min. The GO was further synthesized from the as-carbonized materials using the ‘improved synthesis of graphene oxide’ method. Subsequently, the GO was reduced by low-temperature annealing reduction at 300 °C in a furnace under nitrogen gas for 1 h. The IG/ID ratio calculated from the Raman study increases with the increasing of the degree of the graphitization in the order of rGO from oil palm leaves (rGOOPL) < rGO palm kernel shells (rGOPKS) < rGO commercial graphite (rGOCG) < rGO empty fruit bunches (rGOEFB) with the IG/ID values of 1.06, 1.14, 1.16 and 1.20, respectively. The surface area and pore volume analyses of the as-prepared materials were performed using the Brunauer Emmett Teller-Nitrogen (BET-N2) adsorption-desorption isotherms method. The lower BET surface area of 8 and 15 m2 g−1 observed for rGOCG and rGOOPL, respectively could be due to partial restacking of GO layers and locally-blocked pores. Relatively, this lower BET surface area is inconsequential when compared to rGOPKS and rGOEFB, which have a surface area of 114 and 117 m2 g−1, respectively. PMID:28703757

Method development for the determination of fluorine in water samples via the molecular absorption of strontium monofluoride formed in an electrothermal atomizer

NASA Astrophysics Data System (ADS)

Ozbek, Nil; Akman, Suleyman

The presence of fluorine (F) was detected via the rotational molecular absorption line of diatomic strontium-monofluoride (SrF) generated in the gas phase at 651.187 nm using high-resolution continuum source electrothermal atomic absorption spectrometry. Upon the addition of excess strontium (Sr) as the nitrate, the fluorine in the sample was converted to SrF in the gas phase of a graphite furnace. The effects on the accuracy, precision and sensitivity of variables such as the SrF wavelength, graphite furnace program, amount of Sr, coating of the graphite tube and platform with Zr and Ir and the use of a modifier were investigated and optimized. It was determined that there was no need to use a modifier or to cover the platform/tubes with Zr or Ir. Fluorine concentrations in various water samples (certified waste water, tap water, drinking water and mineral water) were determined using 20 μg of Sr as the molecule-forming reagent and applying a maximum pyrolysis temperature of 800 °C and a molecule-forming temperature of 2200 °C with a heating rate of 2000 °C s- 1. Good linearity was maintained up to 0.1 μg of F. The accuracy and precision of the method were tested by analyzing certified reference wastewater. The results were in good agreement with certified values, and the precision was satisfactory (RSD < 10%). The limit of detection and the characteristic mass for the method were 0.36 ng and 0.55 ng, respectively. Finally, the fluorine concentrations in several drinking water and mineral water samples taken from the market were determined. The results were in good agreement with the values supplied by the producers. No significant differences were found between the results from the linear calibration and standard addition techniques. The method was determined to be simple, fast, accurate and sensitive.

Unusual Enhancement in Intrinsic Thermal Conductivity of Multilayer Graphene by Tensile Strains

DOE PAGES

Kuang, Youdi; Lindsay, Lucas R.; Huang, Baoling

2015-01-01

High basal plane thermal conductivity k of multi-layer graphene makes it promising for thermal management applications. Here we examine the effects of tensile strain on thermal transport in this system. Using a first principles Boltzmann-Peierls equation for phonon transport approach, we calculate the room-temperature in-plane lattice k of multi-layer graphene (up to four layers) and graphite under different isotropic tensile strains. The calculated in-plane k of graphite, finite mono-layer graphene and 3-layer graphene agree well with previous experiments. The dimensional transitions of the intrinsic k and the extent of the diffusive transport regime from mono-layer graphene to graphite are presented.more » We find a peak enhancement of intrinsic k for multi-layer graphene and graphite with increasing strain and the largest enhancement amplitude is about 40%. In contrast the calculated intrinsic k with tensile strain decreases for diamond and diverges for graphene, we show that the competition between the decreased mode heat capacities and the increased lifetimes of flexural phonons with increasing strain contribute to this k behavior. Similar k behavior is observed for 2-layer hexagonal boron nitride systems, suggesting that it is an inherent thermal transport property in multi-layer systems assembled of purely two dimensional atomic layers. This study provides insights into engineering k of multi-layer graphene and boron nitride by strain and into the nature of thermal transport in quasi-two-dimensional and highly anisotropic systems.« less

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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.

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.

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.

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

PubMed

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

2018-03-01

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

Selenium analysis by an integrated microwave digestion-needle trap device with hydride sorption on carbon nanotubes and electrothermal atomic absorption spectrometry determination

NASA Astrophysics Data System (ADS)

Maratta Martínez, Ariel; Vázquez, Sandra; Lara, Rodolfo; Martínez, Luis Dante; Pacheco, Pablo

2018-02-01

An integrated microwave assisted digestion (MW-AD) - needle trap device (NTD) for selenium determination in grape pomace samples is presented. The NTD was filled with oxidized multiwall carbon nanotubes (oxMWCNTS) where Se hydrides were preconcentrated. Determination was carried out by flow injection-electrothermal atomic absorption spectrometry (FI-ETAAS). The variables affecting the system were established by a multivariate design (Plackett Burman), indicating that the following variables significantly affect the system: sample amount, HNO3 digestion solution concentration, NaBH4 volume and elution volume. A Box-Behnken design was implemented to determine the optimized values of these variables. The system improved Se atomization in the graphite furnace, since only trapped hydrides reached the graphite furnace, and the pyrolysis stage was eliminated according to the aqueous matrix of the eluate. Under optimized conditions the system reached a limit of quantification of 0.11 μg kg- 1, a detection limit of 0.032 μg kg- 1, a relative standard deviation of 4% and a preconcentration factor (PF) of 100, reaching a throughput sample of 5 samples per hour. Sample analysis show Se concentrations between 0.34 ± 0.03 μg kg- 1 to 0.48 ± 0.03 μg kg- 1 in grape pomace. This system provides minimal reagents and sample consumption, eliminates discontinuous stages between samples processing reaching a simpler and faster Se analysis.

Graphite for the nuclear industry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Burchell, T.D.; Fuller, E.L.; Romanoski, G.R.

Graphite finds applications in both fission and fusion reactors. Fission reactors harness the energy liberated when heavy elements, such as uranium or plutonium, fragment or fission''. Reactors of this type have existed for nearly 50 years. The first nuclear fission reactor, Chicago Pile No. 1, was constructed of graphite under a football stand at Stagg Field, University of Chicago. Fusion energy devices will produce power by utilizing the energy produced when isotopes of the element hydrogen are fused together to form helium, the same reaction that powers our sun. The role of graphite is very different in these two reactormore » systems. Here we summarize the function of the graphite in fission and fusion reactors, detailing the reasons for their selection and discussing some of the challenges associated with their application in nuclear fission and fusion reactors. 10 refs., 15 figs., 1 tab.« less

Combustion in a multiburner furnace with selective flow of oxygen

DOEpatents

Bool, III, Lawrence E.; Kobayashi, Hisashi

2004-03-02

Improved operational characteristics such as improved fuel efficiency, reduction of NOx formation, reduction of the amount of unburned carbon in the ash, and lessened tendency to corrosion at the tube wall, in a multi-burner furnace are obtained by reducing the flow rate of combustion air to the burners and selectively individually feeding oxidant to only some of the burners.

Furnace Cyclic Behavior of Plasma-Sprayed Zirconia-Yttria and Multi-Component Rare Earth Oxide Doped Thermal Barrier Coatings

NASA Technical Reports Server (NTRS)

Zhu, Dongming; Nesbitt, James A.; McCue, Terry R.; Barrett, Charles A.; Miller, Robert A.

2002-01-01

Ceramic thermal barrier coatings will play an increasingly important role in advanced gas turbine engines because of their ability to enable further increases in engine temperatures. However, the coating performance and durability become a major concern under the increasingly harsh thermal cycling conditions. Advanced zirconia- and hafnia-based cluster oxide thermal barrier coatings with lower thermal conductivity and improved thermal stability are being developed using a high-heat-flux laser-rig based test approach. Although the new composition coatings were not yet optimized for cyclic durability, an initial durability screening of numerous candidate coating materials was carried out using conventional furnace cyclic tests. In this paper, furnace thermal cyclic behavior of the advanced plasma-sprayed zirconia-yttria-based thermal barrier coatings that were co-doped with multi-component rare earth oxides was investigated at 1163 C using 45 min hot cycles. The ceramic coating failure mechanisms were studied by using scanning electron microscopy combined with X-ray diffraction phase analysis after the furnace tests. The coating cyclic lifetime will be discussed in relation to coating phase structures, total dopant concentrations, and other properties.

Electric furnace dust: Can you bury the hazard?

DOE Office of Scientific and Technical Information (OSTI.GOV)

McManus, G.J.

1996-04-01

Electric furnace waste treatment is moving into high gear, but the exact direction is unclear. On one hand, there is a trend toward complete recycling of the dust captured in furnace baghouses. Iron units as well as zinc and other elements are being reclaimed. On the other side, recent actions by regulators indicate recycling may not be required at all. With the correct chemical stabilization, it appears, dust may simply be placed in ordinary landfill. This paper describes three processes for waste treatment of furnace dust: Super Detox, a process for zinc removal from galvanized scrap before melting, and themore » INMETCO process.« less

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.

Multi-Physics Simulation of TREAT Kinetics using MAMMOTH

DOE Office of Scientific and Technical Information (OSTI.GOV)

DeHart, Mark; Gleicher, Frederick; Ortensi, Javier

With the advent of next generation reactor systems and new fuel designs, the U.S. Department of Energy (DOE) has identified the need for the resumption of transient testing of nuclear fuels. DOE has decided that the Transient Reactor Test Facility (TREAT) at Idaho National Laboratory (INL) is best suited for future testing. TREAT is a thermal neutron spectrum nuclear test facility that is designed to test nuclear fuels in transient scenarios. These specific fuels transient tests range from simple temperature transients to full fuel melt accidents. The current TREAT core is driven by highly enriched uranium (HEU) dispersed in amore » graphite matrix (1:10000 U-235/C atom ratio). At the center of the core, fuel is removed allowing for the insertion of an experimental test vehicle. TREAT’s design provides experimental flexibility and inherent safety during neutron pulsing. This safety stems from the graphite in the driver fuel having a strong negative temperature coefficient of reactivity resulting from a thermal Maxwellian shift with increased leakage, as well as graphite acting as a temperature sink. Air cooling is available, but is generally used post-transient for heat removal. DOE and INL have expressed a desire to develop a simulation capability that will accurately model the experiments before they are irradiated at the facility, with an emphasis on effective and safe operation while minimizing experimental time and cost. At INL, the Multi-physics Object Oriented Simulation Environment (MOOSE) has been selected as the model development framework for this work. This paper describes the results of preliminary simulations of a TREAT fuel element under transient conditions using the MOOSE-based MAMMOTH reactor physics tool.« less

The contents and distributions of cadmium, mercury, and lead in Usnea antarctica lichens from Solorina Valley, James Ross Island (Antarctica).

PubMed

Zvěřina, Ondřej; Coufalík, Pavel; Barták, Miloš; Petrov, Michal; Komárek, Josef

2017-12-11

Lichens are efficient and cost-effective biomonitors of the environment. Their geographic distribution together with their slow growth rate enable investigation of the deposition patterns of various elements and substances. In this research, levels of cadmium, lead, and mercury in Usnea antarctica lichens in the area of James Ross Island, Antarctica, were investigated. The lichens were microwave-digested, and the metals were determined by means of atomic absorption spectrometry with graphite furnace and a direct mercury analyzer. Median total contents of Cd, Hg, and Pb were 0.04, 0.47, and 1.6 mg/kg in whole lichens, respectively. The bottom-up distributions of these metals in the fruticose lichen thalli were investigated, and it was revealed that the accumulation patterns for mercury and lead were opposite to that for cadmium. The probable reason for this phenomenon may lie in the inner structure of thalli. The total contents of metals were comparable with those published for other unpolluted areas of maritime Antarctica. However, this finding was not expected for mercury, since the sampling locality was close to an area with some of the highest mercury contents published for Antarctic lichens. In short, lichens proved their usability as biological monitors, even in harsh conditions. However, the findings emphasize the need to take into account the distributions of elements both in the environment and in the lichen itself.

Metalloproteomics Approach to Analyze Mercury in Breast Milk and Hair Samples of Lactating Women in Communities of the Amazon Basin, Brazil.

PubMed

Cerbino, M R; Vieira, José Cavalcante Souza; Braga, C P; Oliveira, G; Padilha, I F; Silva, T M; Zara, L F; Silva, N J; Padilha, P M

2018-02-01

Mercury is a potentially toxic element that is present in the environment of the Brazilian Amazon and is responsible for adverse health effects in humans. This study sought to assess possible protein biomarkers of mercury exposure in breast milk samples from lactating women in the Madeira and Negro Rivers in the Brazilian Amazon. The mercury content of hair samples of lactating women was determined, and the proteome of breast milk samples was obtained using two-dimensional electrophoresis after protein precipitation with acetone. Mercury measurements of protein spots obtained via protein fractionation were performed by graphite furnace atomic absorption spectrometry (GFAAS), and it was observed that mercury is linked to proteins with molecular masses in the range of 14-26 kDa. The total mercury concentration was also determined by GFAAS in unprocessed milk, lyophilized milk, and protein pellets, with the purpose of determining the mercury mass balance in relation to the concentration of this element in milk and pellets. Approximately 85 to 97% of mercury present in the lyophilized milk from samples of lactating women of the Madeira River is bound in the protein fraction. From lactating women of the Negro River, approximately 49% of the total mercury is bound in the protein fraction, and a difference of 51% is bound in the lipid fraction.

Applications of X Radiography to Examination of Nuclear Graphite; APPLICATIONS DE LA RADIOGRAPHIE X A L'EXAMEN DU GRAPHITE NUCLEAIRE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Magnier, P.

1960-06-01

A technique which determines some important elements in the structure of graphite, osme dislocation lines, the presence of some dense impurities, and the local decreases in density, which develop in the course of oxidation, is described. (P.C.H.)

Multiple-element semiquantitative analysis of one-milligram geochemical samples by D.C. arc emission spectrography

USGS Publications Warehouse

Rait, N.

1981-01-01

A modified method is described for a 1-mg sample multi-element semiquantitative spectrographic analysis. This method uses a direct-current arc source, carbon instead of graphite electrodes, and an 80% argon-20% oxygen atmosphere instead of air. Although this is a destructive method, an analysis can be made for 68 elements in all mineral and geochemical samples. Carbon electrodes have been an aid in improving the detection limits of many elements. The carbon has a greater resistance to heat conductance and develops a better tip, facilitating sample volatilization and counter balancing the cooling effect of a flow of the argon-oxygen mixture around the anode. Where such an argon-oxygen atmosphere is used instead of air, the cyanogen band lines are greatly diminished in intensity, and thus more spectral lines of analysis elements are available for use; the spectral background is also lower. The main advantage of using the carbon electrode and the 80% argon-20% oxygen atmosphere is the improved detection limits of 36 out of 68 elements. The detection limits remain the same for 23 elements, and are not as good for only nine elements. ?? 1981.

Continous Monitoring of Melt Composition

NASA Technical Reports Server (NTRS)

Frazer, R. E.; Andrews, T. W.

1984-01-01

Compositions of glasses and alloys analyzed and corrected in real time. Spectral analysis and temperature measurement performed simultaneously on molten material in container, such as open-hearth furnace, crucible or tank of continuous furnace. Speed of analysis makes it possible to quickly measure concentration of volatile elements depleted by prolonged heating.

Nuclear fuel elements and method of making same

DOEpatents

Schweitzer, Donald G.

1992-01-01

A nuclear fuel element for a high temperature gas nuclear reactor that has an average operating temperature in excess of 2000.degree. C., and a method of making such a fuel element. The fuel element is characterized by having fissionable fuel material localized and stabilized within pores of a carbon or graphite member by melting the fissionable material to cause it to chemically react with the carbon walls of the pores. The fissionable fuel material is further stabilized and localized within the pores of the graphite member by providing one or more coatings of pyrolytic carbon or diamond surrounding the porous graphite member so that each layer defines a successive barrier against migration of the fissionable fuel from the pores, and so that the outermost layer of pyrolytic carbon or diamond forms a barrier between the fissionable material and the moderating gases used in an associated high temperature gas reactor. The method of the invention provides for making such new elements either as generally spherically elements, or as flexible filaments, or as other relatively small-sized fuel elements that are particularly suited for use in high temperature gas reactors.

Carbon transfer from magnesia-graphite ladle refractories to ultra-low carbon steel

NASA Astrophysics Data System (ADS)

Russo, Andrew Arthur

Ultra-low carbon steels are utilized in processes which require maximum ductility. Increases in interstitial carbon lower the ductility of steel; therefore, it is important to examine possible sources of carbon. The refractory ladle lining is one such source. Ladle refractories often contain graphite for its desirable thermal shock and slag corrosion resistance. This graphite is a possible source of carbon increase in ultra-low carbon steels. The goal of this research is to understand and evaluate the mechanisms by which carbon transfers to ultra-low carbon steel from magnesia-graphite ladle refractory. Laboratory dip tests were performed in a vacuum induction furnace under an argon atmosphere to investigate these mechanisms. Commercial ladle refractories with carbon contents between 4-12 wt% were used to investigate the effect of refractory carbon content. Slag-free dip tests and slag-containing dip tests with varying MgO concentrations were performed to investigate the influence of slag. Carbon transfer to the steel was controlled by steel penetrating into the refractory and dissolving carbon in dip tests where no slag was present. The rate limiting step for this mechanism is convective mass transport of carbon into the bulk steel. No detectable carbon transfer occurred in dip tests with 4 and 6 wt%C refractories without slag because no significant steel penetration occurred. Carbon transfer was controlled by the corrosion of refractory by slag in dip tests where slag was present.

Effect of Outside Combustion Air on Gas Furnace Efficiency.

DTIC Science & Technology

1981-10-15

Support Agency REPORT FESA-TS-2104 EFFECT OF OUTSIDE COMBUSTION AIR ON GAS FURNACE EFFICIENCY THOMAS E. BRISBANE Q KATHLEEN L. HANCOCK u JOHNS - MANVILLE SALES...and Dilution Air With No Furnace Setback. 93 AO-A113 4~84 . JOHNS - MANVILLE SALES CORP DENVER CO RESEARCH AND OEV--ETC F/6 13/ 1 EFFECT OF OUTSIDE...NUMBER(S) Thomas E. Brisbane, Kathleen L. Hancock DAAK 70-78-D-0002 9. PERFORMING ORGANIZATION NAME AND ADDRESS 1O. PROGRAM ELEMENT. PR.;ECT, TASK Johns

Three-dimensional heat transfer effects during the growth of LiCaAlF 6 in a modified Bridgman furnace

NASA Astrophysics Data System (ADS)

Brandon, Simon; Derby, Jeffrey J.; Atherton, L. Jeffrey; Roberts, David H.; Vital, Russel L.

1993-09-01

A novel process modification, the simultaneous growth of three cylindrical Cr:LiCaAlf 6 (Cr:LiCAF) crystals grown from a common seed in a vertical Bridgman furnace of rectangular cross section, is assessed using computational modeling. The analysis employs the FIDAP finite-element package and accounts for three-dimensional, steady-state, conductive heat transfer throughout the system. The induction heating system is rigorously simulated via solution of Maxwell's equations. The implementation of realistic thermal boundary conditions and furnace details is shown to be important. Furnace design features are assessed through calculations, and simulations indicate expected growth conditions to be favorable. In addition, the validity of using ampoules containing "dummy" charges for experimental furnace characterization measurements is examined through test computations.

Elements of the electric arc furnace's environmental management

NASA Astrophysics Data System (ADS)

Ioana, Adrian; Semenescu, Augustin; Costoiu, Mihnea; Marcu, Dragoş

2017-12-01

The paper presents a theoretical and experimental analysis of the polluting generating mechanisms for steel making in the Electric Arc Furnaces (EAF). The scheme for the environment's polluting system through the EAF is designed and presented in this paper. The ecological experimenting consisted of determining by specialized measures of the dust percentage in the evacuated gases from the EAF and of thereof gas pollutants. From the point of view of reducing the impact on the environment, the main problem of the electric arc furnace (EAF) is the optimization of the powder collecting from the process gases, both from the furnace and from the work-area. The paper deals with the best dependence between the aggregate's constructive, functional and technological factors, which are necessary for the furnace's ecologization and for its energetically-technologically performances increasing.

An ecological risk investigation of marine sediment from the northern Mediterranean coasts (Aegean Sea) using multiple methods of pollution determination.

PubMed

Tunca, Evren; Aydın, Mehmet; Şahin, Ülkü Alver

2018-03-01

The aim of this study is an assessment of metal pollution levels in Aegean Sea sediment. Sediment samples collected from 7 different locations (Yeniköy, Edremit, Ayvalık, Dikili, Aliağa, Hekimadası, and Ildır) along the northern Mediterranean region of Turkey were investigated for 11 elements (Cu, Fe, Zn, V, Cd, Ni, As, Pb, Mn, Co, and Cr). Graphite furnace atomic absorption spectrophotometry (GFAAS) and flame atomic absorption spectrophotometry (FAAS) were used for elemental analysis. The findings were evaluated with sediment assessment methods by taking two different values as a reference and then investigating the adverse biological effects of elemental profiles on living organisms. Pb, Mn, As, Cd, and Cr concentrations were within a moderate to significant range in terms of contamination factor [Formula: see text]), albeit varying according to reference and location. The most problematic region and elements regarding the enrichment factor (EF) was Ayvalık and As, Ni, Cu, Pb, Co, and Cd. However, according to the EF, the anthropogenic effect was not at an alarming level. This was further supported by the results of the geoaccumulation index (Igeo). The findings of the modified degree of contamination (mC d ) and the pollution load index (PLI) suggested that the accumulation was greatest in Ayvalık, and the least in Hekimadası and Ildır. The location with the highest elemental total toxic unit (ΣTU) was Edremit. The effect of the existing element profile on organisms was 21% in this location when the mean effect range-median quotient (m-ERM-q) was considered. As and Ni concentrations in all stations were found to be higher than threshold effect level (TEL) and Effect Range Low (ERL). Ni levels in Edremit exceeded the probable effect level (PEL) and Effect Range Median (ERM). Toxic unit (TU) values of these two elements in all stations ranged from 59.30 to 80.43%.

Recapturing Graphite-Based Fuel Element Technology for Nuclear Thermal Propulsion

DOE Office of Scientific and Technical Information (OSTI.GOV)

Trammell, Michael P; Jolly, Brian C; Miller, James Henry

ORNL is currently recapturing graphite based fuel forms for Nuclear Thermal Propulsion (NTP). This effort involves research and development on materials selection, extrusion, and coating processes to produce fuel elements representative of historical ROVER and NERVA fuel. Initially, lab scale specimens were fabricated using surrogate oxides to develop processing parameters that could be applied to full length NTP fuel elements. Progress toward understanding the effect of these processing parameters on surrogate fuel microstructure is presented.

The effect of Si-contents on the impact properties and dynamic graphite growth for cast iron QT400-18L

NASA Astrophysics Data System (ADS)

Lipeng, Jiang; Yingdong, Qu; Rongde, Li

2018-03-01

Low temperature impact test of QT400-18L ductile iron was investigated. The microstructure and fracture morphology were analyzed by the optical microscope and scanning electron microscope. The effect of different Si content on the graphite growth by liquid quenching method was discussed. There are the highest impact energies for the cast iron with 2.1% of Si over the whole investigated temperature range (‑60 to 20 °C). With the Si element addition increased from 1.9% to 2.1%, the graphite nodulizing grade of QT400 18L is increased from 5 to 7. However the graphite nodulizing grade is reduced from 7 to 6 with Si content increasing from 2.1% to 2.3%. When the Si element addition is exceed 2.1%, the excess of Si content also leads to abnormal graphite. The large size of the abnormal graphite is equivalent to a larger microcrack in the ferrite matrix, and it is helpful for the crack propagation. Large size of abnormal graphite not only destroyed the continuity of ferritic matrix, but also it creates the stress concentration in the surrounding.

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

NASA Technical Reports Server (NTRS)

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

1990-01-01

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

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

NASA Astrophysics Data System (ADS)

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

1990-01-01

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

Determination of rare earth and concomitant elements in magnesium alloys by inductively coupled plasma optical emission spectrometry.

PubMed

Fariñas, Juan C; Rucandio, Isabel; Pomares-Alfonso, Mario S; Villanueva-Tagle, Margarita E; Larrea, María T

2016-07-01

An Inductively Coupled Plasma Optical Emission Spectrometry method for simultaneous determination of Al, Ca, Cu, Fe, In, Mn, Ni, Si, Sr, Y, Zn, Zr and rare earth elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu) in magnesium alloys, including the new rare earth elements-alloyed magnesium, has been developed. Robust conditions have been established as nebulizer argon flow rate of 0.5mLmin(-1) and RF incident power of 1500W, in which matrix effects were significantly reduced around 10%. Three acid digestion procedures were performed at 110°C in closed PFA vessels heated in an oven, in closed TFM vessels heated in a microwave furnace, and in open polypropylene tubes with reflux caps heated in a graphite block. The three digestion procedures are suitable to put into solution the magnesium alloys samples. From the most sensitive lines, one analytical line with lack or low spectral interferences has been selected for each element. Mg, Rh and Sc have been studied as internal standards. Among them, Rh was selected as the best one by using Rh I 343.488nm and Rh II 249.078nm lines as a function of the analytical lines. The trueness and precision have been established by using the Certified Reference Material BCS 316, as well as by means of recovery studies. Quantification limits were between 0.1 and 9mgkg(-1) for Lu and Pr, respectively, in a 2gL(-1) magnesium matrix solution. The method developed has been applied to the commercial alloys AM60, AZ80, ZK30, AJ62, WE54 and AE44. Copyright © 2016 Elsevier B.V. All rights reserved.

Data on metals (Zn, Al, Sr, and Co) and metalloid (As) concentration levels of ballast water in commercial ships entering Bushehr port, along the Persian Gulf.

PubMed

Soleimani, Farshid; Dobaradaran, Sina; Hayati, Abdolreza; Khorsand, Maryam; Keshtkar, Mozhgan

2016-12-01

In this article, we determined the concentration levels of metals including Zn, Al, Sr, and Co and metalloid of As of ballast water in commercial ships entering Bushehr port, along the Persian Gulf. Ballast water samples were taken from commercial ships entering Bushehr port from 34 ports around the world during 15 February and 25 August 2016. The concentration levels of metals and metalloid were determined by using a graphite furnace absorption spectrometer (AAS).

Toxic metals in imported fruits and vegetables marketed in Kuwait

DOE Office of Scientific and Technical Information (OSTI.GOV)

Husain, A.; Baroon, Z.; Al-Khalafawi, M.

1995-12-31

The concentration of lead, cadmium, and mercury in 134 samples of imported fruits and vegetables marketed in Kuwait were determined using an atomic absorption spectrophotometer with a graphite furnace and the cold vapor technique. Results obtained showed that the concentration of these metal ions in most cases did not exceed the maximum permissible concentration of metals in fresh fruits and vegetables as restricted by some countries. Only a few samples of fruits and vegetables contained levels of mercury, cadmium, and lead which exceeded these maximum permissible levels.

An induction furnace for the determination of cadmium in solutions and zinc-base metals by atomic-absorption spectroscopy.

PubMed

Headridge, J B; Smith, D R

1971-03-01

An induction furnace coupled to a Unicam SP90 atomic-absorption spectrophotometer is described for the determination of traces of volatile elements in solutions and volatile matrices. The apparatus has been used to obtain calibration graphs for 1-20 and 50-750 ng of cadmium in microl-volumes of solution, the 228.8 and 326.2 nm resonance lines respectively being used, and to determine cadmium in 5-mg samples of zinc-base metals within the concentration range 5-400 microg g by using the less sensitive 326-2-nm line. A furnace temperature of 1,350 degrees was used. Data on accuracy and precision are presented. The apparatus could readily be used to determine trace elements in volatile materials at concentrations of 10-1000 ng/g .

Reducing Thermal Conduction In Acoustic Levitators

NASA Technical Reports Server (NTRS)

Lierke, Ernst G.; Leung, Emily W.; Bhat, Balakrishna T.

1991-01-01

Acoustic transducers containing piezoelectric driving elements made more resistant to heat by reduction of effective thermal-conductance cross sections of metal vibration-transmitting rods in them, according to proposal. Used to levitate small objects acoustically for noncontact processing in furnaces. Reductions in cross sections increase amplitudes of transmitted vibrations and reduce loss of heat from furnaces.

Fiber glass pulling. [in space

NASA Technical Reports Server (NTRS)

Workman, Gary L.

1987-01-01

Experiments were conducted to determine the viability of performing containerless glass fiber pulling in space. The optical transmission properties and glass-forming capabilities of the heavy metal fluorides are reviewed and the acoustic characteristics required for a molten glass levitation system are examined. The design limitations of, and necessary modifications to the acoustic levitation furnace used in the experiments are discussed in detail. Acoustic levitator force measurements were performed and a thermal map of the furnace was generated from thermocouple data. It was determined that the thermal capability of the furnace was inadequate to melt a glass sample in the center. The substitution of a 10 KW carbon monoxide laser for the original furnace heating elements resulted in improved melt heating.

THE PARTITIONING OF ALLOYING ELEMENTS IN MALLEABLE IRONS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sandoz, G.

1958-12-23

The partitioning of a number of alloying elements between the cementite and austenite phases of irons during first-stage graphitization has been determined. For the most part, the data were obtained by chemical analyses of the cementite chemically extracted from irons quenched after selected periods at l650 F. Spot checks of these results and some explorations of alloy distribution in the matrix were made with the electron probe microanalyzer. The results show that the elements V, Cr, Mo, and Mn (not combined with S) concentrate in the cementite phase and may further enrich in this phase during graphitization. Small but measurablemore » amounts of the elements Si, Cu, Ni, Co, and Al are also found in the cementite phase. Sulfur dissolves partially in the cementite phase but is removed insofar as MnS is formed. The finding of significant amounts of every alloying element investigated in the cementite phase suggests that the mechanism by which alloying elements influenee graphitization kinetics may involve a change in the thermodynamic stability of the cementite phase. (auth)« less

Elemental Metals or Oxides Distributed on a Carbon Substrate or Self-Supported and the Manufacturing Process Using Graphite Oxide as Template

NASA Technical Reports Server (NTRS)

Hung, Ching-Chen (Inventor)

1999-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a percursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen. This intermediary product can be further processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Elemental Metals or Oxides Distributed on a Carbon Substrate or Self-Supported and the Manufacturing Process Using Graphite Oxide as Template

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh (Inventor)

1999-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen. This intermediary product can be further processed by direct exposure to carbonate-solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Two-temperature synthesis of non-linear optical compound CdGeAs2

NASA Astrophysics Data System (ADS)

Zhu, Chongqiang; Verozubova, G. A.; Mironov, Yuri P.; Lei, Zuotao; Song, Liangcheng; Ma, Tianhui; Okunev, A. O.; Yang, Chunhui

2016-12-01

In this work, we report on a new approach to synthesize large-scale nonlinear optical chalcopyrite compound CdGeAs2 (cadmium germanium arsenide), in which the arsenic (As) precursor and the mixture of the cadmium (Cd) and the germanium (Ge) were separated in two distinct temperature-defined zones of a furnace. Through probing the intermediate product prepared at pre-set temperature points of hot-zone area, it was revealed that the ternary compound CdGeAs2 was formed through chemical reactions among Cd3As2, CdAs2, GeAs, GeAs2 and Ge. A new intermediate crystalline compound, with determined crystal parameter c=0.9139 nm and unknown a parameter, was identified when the temperature of the mixture of Cd and Ge was set to 680 °C, which, however, disappeared when the temperature was set to 770 °C, yielding pure CdGeAs2 product. Most likely, the identified new intermediate compound has layered graphite-like structure. Moreover, we show that the described two-temperature synthesis method allows us to produce near 250 g CdGeAs2 product during one run in a horizontal furnace and 500 g in a tilted horizontal furnace with rotated reactor.

The synthesis of graphene at different deposition time from palm oil via thermal chemical vapor deposition

NASA Astrophysics Data System (ADS)

Salifairus, M. J.; Soga, T.; Alrokayan, Salman A. H.; Khan, Haseeb A.; Rusop, M.

2018-05-01

The basic building of graphitic materials is graphene that can range from zero-dimensional to three-dimensional. Graphene is a single atomic layer of sp2 bonded carbon atoms. It becomes most potential new materials to replace silicon due to its fascinating properties. In this study, the graphene growth was observed at different deposition time. The 1cm x 1cm polycrystalline nickel substrate was cleaned by etching process. The palm oil, carbon source, was placed in the precursor furnace and the nickel substrate was placed in the second furnace (deposition furnace). The palm oil will mix with Argon and Hydrogen gas was used as carrier gas in the CVD under certain temperature and pressure to undergo pyrolysis process. The deposition temperature was set at 900 °C and the deposition time was varied from 5 - 60 minutes. The graphene was growth at ambient pressure in the CVD system. Raman spectrometer and atomic force microscopy revealed the structural properties and surface topography of the grapheme on the nickel substrate. The D, G and 2D band appear approximately at 1378 cm-1, 1580 cm-1 and 2696 cm-1. It can be concluded that the graphene has successfully synthesized at different deposition time.

Application of Argonne's Glass Furnace Model to longhorn glass corporation oxy-fuel furnace for the production of amber glass.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Golchert, B.; Shell, J.; Jones, S.

2006-09-06

The objective of this project is to apply the Argonne National Laboratory's Glass Furnace Model (GFM) to the Longhorn oxy-fuel furnace to improve energy efficiency and to investigate the transport of gases released from the batch/melt into the exhaust. The model will make preliminary estimates of the local concentrations of water, carbon dioxide, elemental oxygen, and other subspecies in the entire combustion space as well as the concentration of these species in the furnace exhaust gas. This information, along with the computed temperature distribution in the combustion space may give indications on possible locations of crown corrosion. An investigation intomore » the optimization of the furnace will be performed by varying several key parameters such as the burner firing pattern, exhaust number/size, and the boost usage (amount and distribution). Results from these parametric studies will be analyzed to determine more efficient methods of operating the furnace that reduce crown corrosion. Finally, computed results from the GFM will be qualitatively correlated to measured values, thus augmenting the validation of the GFM.« less

Effect of Elevated Pressure on the Heat Transfer and Power Requirements During Bridgman Growth of PMN-PT Crystals

NASA Technical Reports Server (NTRS)

Bune, Andris; Ostrogorsky, Aleksandar; Marin, Carlos; Nicoara, Irina; Rose, M. Franklin (Technical Monitor)

2000-01-01

Performance of the furnace during Bridgman growth of the lead magnesium niobate-lead titanate crystal (PMN-PT) is analyzed. PMN-PT is electrostrictive ceramic that has near ideal strain-voltage function. Furthermore piezoelectric (2000 to 2300 pC/N) and coupling (92 to 95%) constants are exceptionally good. Due to these properties PMN-PT has wide range of applications - from sonars to transducers in a high precision optical systems. In this research first attempt to crystallize PMN-PT in a Mellen type vertical Bridgman furnace was not successful, as melting temperature of precursor materials was not achieved. At this point choice was between building a new more powerful facility or finding ways to enhance performance of the existing furnace. Besides adjusting power supply to the individual heating elements, redesigning ampoule holding cartridge and improving furnace insulation one more radical improvement was proposed. The entire furnace was placed into the high pressure chamber. Further experiments confirmed that temperature inside the furnace was increased sufficiently to melt precursor materials to obtain PMN-PT. Numerical modeling is undertaken to find limitations of this technique and to predict temperature distribution inside the ampoule. It is of interest also to account for main factors contributing to a higher temperatures achieved in the furnace under the higher pressure (up to 10 atm.). Numerical model of the furnace is based on general purpose finite - element code FIDAP and on previous efforts to model Bridgman type furnace with multiply heaters. In order to account for all heat transfer mechanism involved - conduction, convection and radiation - different parts of the furnace are modeled in accordance with expected dominant mode of heat transfer - conduction in the solid parts, conduction and radiation in the ampoule, gas convection and conduction in the furnace openings complemented with wall-to-wall radiation. Because of these complicating factors, dimensional rather than non-dimensional modeling is performed using steady-state 2-D and 3-D models. Particular attention is paid to the modeling of radiation in a semitransparent material of ampoule 7 sapphire. The radiation model is validated by solving realistic test problem - conduction and radiation heat transfer in the fused quartz. Results are in agreement with both experimental and analytical data.

Multipurpose electroslag remelting furnace for modern energy and heavy engineering industry

NASA Astrophysics Data System (ADS)

Dub, A. V.; Dub, V. S.; Kriger, Yu. N.; Levkov, L. Ya.; Shurygin, D. A.; Kissel'man, M. A.; Nekhamin, C. M.; Chernyak, A. I.; Bessonov, A. V.; Kamantsev, S. V.; Sokolov, S. O.

2012-12-01

In 2011, a unique complex based on a multipurpose unit-type electroslag remelting (ESR) furnace is created to meet the demand for large high-quality solid and hollow billets for the products of power, atomic, petrochemical, and heavy machine engineering. This complex has modern low-frequency power supplies with a new control level that ensure a high homogeneity and quality of the billets and an increase in the engineering-and-economical performance of the production. A unique pilot ESR furnace is erected to adjust technological conditions and the main control system elements.

Model reduction for experimental thermal characterization of a holding furnace

NASA Astrophysics Data System (ADS)

Loussouarn, Thomas; Maillet, Denis; Remy, Benjamin; Dan, Diane

2017-09-01

Vacuum holding induction furnaces are used for the manufacturing of turbine blades by loss wax foundry process. The control of solidification parameters is a key factor for the manufacturing of these parts. The definition of the structure of a reduced heat transfer model with experimental identification through an estimation of its parameters is required here. Internal sensors outputs, together with this model, can be used for assessing the thermal state of the furnace through an inverse approach, for a better control. Here, an axisymmetric furnace and its load have been numerically modelled using FlexPDE, a finite elements code. The internal induction heat source as well as the transient radiative transfer inside the furnace are calculated through this detailed model. A reduced lumped body model has been constructed to represent the numerical furnace. The model reduction and the estimation of the parameters of the lumped body have been made using a Levenberg-Marquardt least squares minimization algorithm, using two synthetic temperature signals with a further validation test.

Determination of fluorine and chlorine in geological materials by induction furnace pyrohydrolysis and standard-addition ion-selective electrode measurement.

PubMed

Rice, T D

1988-03-01

Fluorine and chlorine in geological materials are volatilized by pyrohydrolysis at about 1150 degrees in a stream of oxygen (1000 ml/min) plus steam in an induction furnace. The catalyst is a 7:2:1 mixture of silica gel, tungstic oxide and potassium dihydrogen phosphate. The sample/catalyst mixture is pyrohydrolysed in a re-usable alumina crucible (already containing four drops of 1 + 3 phosphoric acid) inserted in a silica-enclosed graphite crucible. The absorption solution is buffered at pH 6.5 and spiked with 1.6 mug of fluoride and 16 mug of chloride per g of solution, to ensure rapid and linear electrode response during subsequent standard-addition measurement. The simple plastic absorption vessel has 99.5% efficiency. The 3s limits of detection are 5-10 mug/g and 40-100 mug/g for fluorine and chlorine respectively. The procedure is unsuitable for determining chlorine in coal.

HIGH TEMPERATURE TREATMENT OF INTERMEDIATE-LEVEL RADIOACTIVE WASTES - SIA RADON EXPERIENCE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sobolev, I.A.; Dmitriev, S.A.; Lifanov, F.A.

2003-02-27

This review describes high temperature methods of low- and intermediate-level radioactive waste (LILW) treatment currently used at SIA Radon. Solid and liquid organic and mixed organic and inorganic wastes are subjected to plasma heating in a shaft furnace with formation of stable leach resistant slag suitable for disposal in near-surface repositories. Liquid inorganic radioactive waste is vitrified in a cold crucible based plant with borosilicate glass productivity up to 75 kg/h. Radioactive silts from settlers are heat-treated at 500-700 0C in electric furnace forming cake following by cake crushing, charging into 200 L barrels and soaking with cement grout. Variousmore » thermochemical technologies for decontamination of metallic, asphalt, and concrete surfaces, treatment of organic wastes (spent ion-exchange resins, polymers, medical and biological wastes), batch vitrification of incinerator ashes, calcines, spent inorganic sorbents, contaminated soil, treatment of carbon containing 14C nuclide, reactor graphite, lubricants have been developed and implemented.« less

AMTEC powered residential furnace and auxiliary power

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ivanenok, J.F. III; Sievers, R.K.

1996-12-31

Residential gas furnaces normally rely on utility grid electric power to operate the fans and/or the pumps used to circulate conditioned air or water and they are thus vulnerable to interruptions of utility grid service. Experience has shown that such interruptions can occur during the heating season, and can lead to serious consequences. A gas furnace coupled to an AMTEC conversion system retains the potential to produce heat and electricity (gas lines are seldom interrupted during power outages), and can save approximately $47/heating season compared to a conventional gas furnace. The key to designing a power system is understanding, andmore » predicting, the cell performance characteristics. The three main processes that must be understood and modeled to fully characterize an AMTEC cell are the electro-chemical, sodium vapor flow, and heat transfer. This paper will show the results of the most recent attempt to model the heat transfer in a multi-tube AMTEC cell and then discusses the conceptual design of a self-powered residential furnace.« less

Colloidal-facilitated transport of inorganic contaminants in ground water: part 1, sampling considerations

USGS Publications Warehouse

Puls, Robert W.; Eychaner, James H.; Powell, Robert M.

1996-01-01

Investigations at Pinal Creek, Arizona, evaluated routine sampling procedures for determination of aqueous inorganic geochemistry and assessment of contaminant transport by colloidal mobility. Sampling variables included pump type and flow rate, collection under air or nitrogen, and filter pore diameter. During well purging and sample collection, suspended particle size and number as well as dissolved oxygen, temperature, specific conductance, pH, and redox potential were monitored. Laboratory analyses of both unfiltered samples and the filtrates were performed by inductively coupled argon plasma, atomic absorption with graphite furnace, and ion chromatography. Scanning electron microscopy with Energy Dispersive X-ray was also used for analysis of filter particulates. Suspended particle counts consistently required approximately twice as long as the other field-monitored indicators to stabilize. High-flow-rate pumps entrained normally nonmobile particles. Difference in elemental concentrations using different filter-pore sizes were generally not large with only two wells having differences greater than 10 percent in most wells. Similar differences (>10%) were observed for some wells when samples were collected under nitrogen rather than in air. Fe2+/Fe3+ ratios for air-collected samples were smaller than for samples collected under a nitrogen atmosphere, reflecting sampling-induced oxidation.

A Comparison of Materials Issues for Cermet and Graphite-Based NTP Fuels

NASA Technical Reports Server (NTRS)

Stewart, Mark E.; Schnitzler, Bruce G.

2013-01-01

This paper compares material issues for cermet and graphite fuel elements. In particular, two issues in NTP fuel element performance are considered here: ductile to brittle transition in relation to crack propagation, and orificing individual coolant channels in fuel elements. Their relevance to fuel element performance is supported by considering material properties, experimental data, and results from multidisciplinary fluid/thermal/structural simulations. Ductile to brittle transition results in a fuel element region prone to brittle fracture under stress, while outside this region, stresses lead to deformation and resilience under stress. Poor coolant distribution between fuel element channels can increase stresses in certain channels. NERVA fuel element experimental results are consistent with this interpretation. An understanding of these mechanisms will help interpret fuel element testing results.

Sulfate Fining Chemistry in Oxidized and Reduced Soda-Lime-Silica Glasses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Matyas, Josef; Hrma, Pavel R.

2005-05-13

Various reducing agents were used and their additions were varied to (1) increase glass quality through eliminating defects from silica scum, (2) decrease SOx emissions through changing the kind and quantity of reducing agents, and (3) improve production efficiency through increased flexibility of glass redox control during continuous processing. The work included measuring silica sand dissolution and sulfate decomposition in melts from glass batches. Glass batches were heated at a temperature-increase rate deemed similar to that experienced in the melting furnace. The sulfate decomposition kinetics was investigated with thermogravimetric analysis-differential thermal analysis and evolved gas analysis. Sulfur concentrations in glassesmore » quenched at different temperatures were determined using X-ray fluorescence spectroscopy. The distribution of residual sand (that which was not dissolved during the initial batch reactions) in the glass was obtained as a function of temperature with optical microscopy in thin-sections of melts. The fraction of undissolved sand was measured with X-ray diffraction. The results of the present study helped Visteon Inc. reduce the energy consumption and establish the batch containing 0.118 mass% of graphite as the best candidate for Visteon glass production. The improved glass batch has a lower potential for silica scum formation and for brown fault occurrence in the final glass product. It was established that bubbles trapped in the melt even at 1450 C have a high probability to be refined when reaching the hot zone in the glass furnace. Furthermore, silica sand does not accumulate at the glass surface and dissolves faster in the batch with graphite than in the batch with carbocite.« less

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.

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.

76 FR 53057 - Change to the Reporting Date for Certain Data Elements Required Under the Mandatory Reporting of...

Federal Register 2010, 2011, 2012, 2013, 2014

2011-08-25

..., blast furnaces, basic oxygen process furnace shops. Lead Production 331419 Primary lead smelting and.... Chapter 5, generally provides that rules may not take effect earlier than 30 days after they are published... behavior and prepare before the final rule takes effect. Because this final rule defers a reporting...

Mesocarbon microbead based graphite for spherical fuel element to inhibit the infiltration of liquid fluoride salt in molten salt reactor

NASA Astrophysics Data System (ADS)

Zhong, Yajuan; Zhang, Junpeng; Lin, Jun; Xu, Liujun; Zhang, Feng; Xu, Hongxia; Chen, Yu; Jiang, Haitao; Li, Ziwei; Zhu, Zhiyong; Guo, Quangui

2017-07-01

Mesocarbon microbeads (MCMB) and quasi-isostatic pressing method were used to prepare MCMB based graphite (MG) for spherical fuel element to inhibit the infiltration of liquid fluoride salt in molten salt reactor (MSR). Characteristics of mercury infiltration and molten salt infiltration in MG were investigated and compared with A3-3 (graphite for spherical fuel element in high temperature gas cooled reactor) to identify the infiltration behaviors. The results indicated that MG had a low porosity about 14%, and an average pore diameter of 96 nm. Fluoride salt occupation of A3-3 (average pore diameter was 760 nm) was 10 wt% under 6.5 atm, whereas salt gain did not infiltrate in MG even up to 6.5 atm. It demonstrated that MG could inhibit the infiltration of liquid fluoride salt effectively. Coefficient of thermal expansion (CTE) of MG lies in 6.01 × 10-6 K-1 (α∥) and 6.15 × 10-6 K-1 (α⊥) at the temperature range of 25-700 °C. The anisotropy factor of MG calculated by CTE maintained below 1.02, which could meet the requirement of the spherical fuel element (below 1.30). The constant isotropic property of MG is beneficial for the integrity and safety of the graphite used in the spherical fuel element for a MSR.

Swedish materials science experiment equipment

NASA Astrophysics Data System (ADS)

Jonsson, R.

1982-09-01

Details of the apparatus and experimentation performed with the Swedish MURMEC (multi-purpose Rocket-borne Materials science Experiment Carrier) and other materials science equipment for sounding rocket and airborne trials are presented. The MURMEC science modules contain four isothermal furnaces, 12 pore formation experiment furnaces, and two gradient furnaces. The modules feature a power system, experimental control, and monitoring sensors. Design details and operational features of each of the furnaces are provided, and results of the first MURMEC flight on-board a Swedish sounding rocket with the PIRAT (Pointed IR Astronomical Telescope) are discussed. Additional tests were performed using a modified NASA F-104 aircraft flown in a parabolic trajectory to produce a 0.3-0.1 g environment for 50-60 sec. Films were made of melting and resolidification processes during nine different flights using three different samples.

Simulation on an optimal combustion control strategy for 3-D temperature distributions in tangentially pc-fired utility boiler furnaces.

PubMed

Wang, Xi-fen; Zhou, Huai-chun

2005-01-01

The control of 3-D temperature distribution in a utility boiler furnace is essential for the safe, economic and clean operation of pc-fired furnace with multi-burner system. The development of the visualization of 3-D temperature distributions in pc-fired furnaces makes it possible for a new combustion control strategy directly with the furnace temperature as its goal to improve the control quality for the combustion processes. Studied in this paper is such a new strategy that the whole furnace is divided into several parts in the vertical direction, and the average temperature and its bias from the center in every cross section can be extracted from the visualization results of the 3-D temperature distributions. In the simulation stage, a computational fluid dynamics (CFD) code served to calculate the 3-D temperature distributions in a furnace, then a linear model was set up to relate the features of the temperature distributions with the input of the combustion processes, such as the flow rates of fuel and air fed into the furnaces through all the burners. The adaptive genetic algorithm was adopted to find the optimal combination of the whole input parameters which ensure to form an optimal 3-D temperature field in the furnace desired for the operation of boiler. Simulation results showed that the strategy could soon find the factors making the temperature distribution apart from the optimal state and give correct adjusting suggestions.

Thermal properties of graphite oxide, thermally reduced graphene and chemically reduced graphene

NASA Astrophysics Data System (ADS)

Jankovský, Ondřej; Sedmidubský, David; Lojka, Michal; Sofer, Zdeněk

2017-07-01

We compared thermal behavior and other properties of graphite oxide, thermally reduced graphene and chemically reduced graphene. Graphite was oxidized according to the Hofmann method using potassium chlorate as oxidizing agent in strongly acidic environment. In the next step, the formed graphite oxide was chemically or thermally reduced yielding graphene. The mechanism of thermal reduction was studied using STA-MS. Graphite oxide and both thermally and chemically reduced graphenes were analysed by SEM, EDS, elemental combustion analysis, XPS, Raman spectroscopy, XRD and BET. These findings will help for the large scale production of graphene with appropriate chemical composition.

Quality control developments for graphite/PMR15 polyimide composites materials

NASA Technical Reports Server (NTRS)

Sheppard, C. H.; Hoggatt, J. T.

1979-01-01

The problem of lot-to-lot and within-lot variability of graphite/PMR-15 prepreg was investigated. The PMR-15 chemical characterization data were evaluated along with the processing conditions controlling the manufacture of PMR-15 resin and monomers. Manufacturing procedures were selected to yield a consistently reproducible graphite prepreg that could be processed into acceptable structural elements.

Tellurium speciation analysis using hydride generation in situ trapping electrothermal atomic absorption spectrometry and ruthenium or palladium modified graphite tubes.

PubMed

Yildirim, Emrah; Akay, Pınar; Arslan, Yasin; Bakirdere, Sezgin; Ataman, O Yavuz

2012-12-15

Speciation of tellurium can be achieved by making use of different kinetic behaviors of Te(IV) and Te(VI) upon their reaction with sodium borohydride using hydride generation. While Te(IV) can form H(2)Te, Te(VI) will not form any volatile species during the course of hydride formation and measurement by atomic absorption spectrometry. Quantitative reduction of Te(VI) was achieved through application of a microwave assisted prereduction of Te(VI) in 6.0 mol/L HCl solution. Enhanced sensitivity was achieved by in situ trapping of the generated H(2)Te species in a previously heated graphite furnace whose surface was modified using Pd or Ru. Overall efficiency for in situ trapping in pyrolytically coated graphite tube surface was found to be 15% when volatile analyte species are trapped for 60s at 300°C. LOD and LOQ values were calculated as 0.086 ng/mL and 0.29 ng/mL, respectively. Efficiency was increased to 46% and 36% when Pd and Ru surface modifiers were used, respectively. With Ru modified graphite tube 173-fold enhancement was obtained over 180 s trapping period with respect to ETAAS; the tubes could be used for 250 cycles. LOD values were 0.0064 and 0.0022 ng/mL for Pd and Ru treated ETAAS systems, respectively, for 180 s collection of 9.6 mL sample solution. Copyright © 2012 Elsevier B.V. All rights reserved.

Production of chlorine from chloride salts

DOEpatents

Rohrmann, Charles A.

1981-01-01

A process for converting chloride salts and sulfuric acid to sulfate salts and elemental chlorine is disclosed. A chloride salt and sulfuric acid are combined in a furnace where they react to produce a sulfate salt and hydrogen chloride. Hydrogen chloride from the furnace contacts a molten salt mixture containing an oxygen compound of vanadium, an alkali metal sulfate and an alkali metal pyrosulfate to recover elemental chlorine. In the absence of an oxygen-bearing gas during the contacting, the vanadium is reduced, but is regenerated to its active higher valence state by separately contacting the molten salt mixture with an oxygen-bearing gas.

Study of multi-kilowatt solar arrays for Earth orbit applications

NASA Technical Reports Server (NTRS)

Patterson, R. E.

1983-01-01

A miniaturized Cassegrainian concentrator (MCC) solar array concept is being developed with the objective of significantly reducing the recurring cost of multikilowatt solar arrays. The desired cost reduction is obtained as a result of using very small high efficiency solar cells in conjuction with low cost optics. The MCC single element concept incident slar radiation is reflected rom a primary parabolic reflector to a secondary hyperbolic reflector and finally to a 4 millimeter diameter solar cell. A light catcher cone is used to improve off axis performance. The solar cell is mounted to a heat fin. An element is approximately 13 millimeters thick which permits efficient launch stowage of the concentrator system panels without complex optical component deployments or retractions. The MCC elements are packed in bays within graphite epoxy frames and are electrically connected into appropriate series-parallel circuits. A MCC sngle element with a 21 sq cm entrance aperture and a 20 efficient, 0.25 sq cm gallium arsenide solar cell has the same power output as 30 sq cm of 11-percent efficiency (at 68 C) silicon solar cells.

Production of fiberglass/metal composite material suitable for building habitat and manufacturing facilities

NASA Technical Reports Server (NTRS)

1987-01-01

The production of a fiberglass/metal composite material suitable for building habitats and manufacturing facilities was the project for Clemson. The concept and development of the knowledge necessary to produce glass fibers originated in the spring semester. During the summer, while at Johnson Space Center, fiberglass from a rock composition similar to ones found at the Apollo 16 site on the moon was successfully produced. The project this year was a continuation of last year's studies. We addressed the following problems which emerged as the work progressed: (1) Methods for coating the fibers with a metal were explored. We manufactured composites in two stages: Glass fibers without any coating on them; and fibers coated with metals as they were made. This proved to be a difficult process. Future activities include using a chemical vapor deposition process on fibers which have been made. (2) A glass furnace was developed which relies primarily on solar energy for melting the glass. The temperature of the melted glass is maintained by electrical means. The design is for 250 kg of glass per day. An electrical engineering student developed a scheme for controlling the melting and manufacturing process from the earth. This was done to minimize the human risk. Graphite refractories are relied on to contain the melt. (3) The glass composition chosen for the project is a relatively pure anorthite which is available in the highland regions of the lunar surface. A major problems with this material is that it melts at a comparatively high temperature. This problem will be solved by using graphite refractory materials for the furnace. The advantage of this glass composition is that it is very stable and does not tend to crystallize. (4) We have also refined the experimental furnace and fiber making machinery which we will be using at Johnson Space Center this summer. We believe that we will be able to draw and coat glass fibers in a vacuum for use in composites. We intend to make and test the mechanical properties of these composites.

Improvement of graphite crystal analyzer for light elements on X-ray fluorescence holography measurement

NASA Astrophysics Data System (ADS)

Happo, Naohisa; Hada, Takuma; Kubota, Atsushi; Ebisu, Yoshihiro; Hosokawa, Shinya; Kimura, Koji; Tajiri, Hiroo; Matsushita, Tomohiro; Hayashi, Kouichi

2018-05-01

Using a graphite crystal analyzer, focused monochromatic fluorescent X-rays can be obtained on an X-ray fluorescence holography (XFH) measurement. To measure the holograms of elements lighter than Ti, we improved a cylindrical-type crystal analyzer and constructed a small C-shaped analyzer. Using the constructed C-shaped analyzer, a Ca Kα hologram of a fluorite single crystal was obtained, from which we reconstructed a clear atomic image. The XFH measurements for the K, Ca, and Sc elements become possible using the presently constructed analyzer.

JACKETED FUEL ELEMENTS FOR GRAPHITE MODERATED REACTORS

DOEpatents

Szilard, L.; Wigner, E.P.; Creutz, E.C.

1959-05-12

Fuel elements for a heterogeneous, fluid cooled, graphite moderated reactor are described. The fuel elements are comprised of a body of natural uranium hermetically sealed in a jacket of corrosion resistant material. The jacket, which may be aluminum or some other material which is non-fissionable and of a type having a low neutron capture cross-section, acts as a barrier between the fissioning isotope and the coolant or moderator or both. The jacket minimizes the tendency of the moderator and coolant to become radioactive and/or contaminated by fission fragments from the fissioning isotope.

Heating element support clip

DOEpatents

Sawyer, William C.

1995-01-01

An apparatus for supporting a heating element in a channel formed in a heater base is disclosed. A preferred embodiment includes a substantially U-shaped tantalum member. The U-shape is characterized by two substantially parallel portions of tantalum that each have an end connected to opposite ends of a base portion of tantalum. The parallel portions are each substantially perpendicular to the base portion and spaced apart a distance not larger than a width of the channel and not smaller than a width of a graphite heating element. The parallel portions each have a hole therein, and the centers of the holes define an axis that is substantially parallel to the base portion. An aluminum oxide ceramic retaining pin extends through the holes in the parallel portions and into a hole in a wall of the channel to retain the U-shaped member in the channel and to support the graphite heating element. The graphite heating element is confined by the parallel portions of tantalum, the base portion of tantalum, and the retaining pin. A tantalum tube surrounds the retaining pin between the parallel portions of tantalum.

Heating element support clip

DOEpatents

Sawyer, W.C.

1995-08-15

An apparatus for supporting a heating element in a channel formed in a heater base is disclosed. A preferred embodiment includes a substantially U-shaped tantalum member. The U-shape is characterized by two substantially parallel portions of tantalum that each have an end connected to opposite ends of a base portion of tantalum. The parallel portions are each substantially perpendicular to the base portion and spaced apart a distance not larger than a width of the channel and not smaller than a width of a graphite heating element. The parallel portions each have a hole therein, and the centers of the holes define an axis that is substantially parallel to the base portion. An aluminum oxide ceramic retaining pin extends through the holes in the parallel portions and into a hole in a wall of the channel to retain the U-shaped member in the channel and to support the graphite heating element. The graphite heating element is confined by the parallel portions of tantalum, the base portion of tantalum, and the retaining pin. A tantalum tube surrounds the retaining pin between the parallel portions of tantalum. 6 figs.

Effect of Carbon Nanotubes Upon Emissions From Cutting and Sanding Carbon Fiber-Epoxy Composites

PubMed Central

Heitbrink, William A.; Lo, Li-Ming

2015-01-01

Carbon nanotubes (CNTs) are being incorporated into structural composites to enhance material strength. During fabrication or repair activities, machining nanocomposites may release CNTs into the workplace air. An experimental study was conducted to evaluate the emissions generated by cutting and sanding on three types of epoxy-composite panels: Panel A containing graphite fibers, Panel B containing graphite fibers and carbon-based mat, and Panel C containing graphite fibers, carbon-based mat, and multi-walled CNTs. Aerosol sampling was conducted with direct-reading instruments, and filter samples were collected for measuring elemental carbon (EC) and fiber concentrations. Our study results showed that cutting Panel C with a band saw did not generate detectable emissions of fibers inspected by transmission electron microscopy but did increase the particle mass, number, and EC emission concentrations by 20% to 80% compared to Panels A and B. Sanding operation performed on two Panel C resulted in fiber emission rates of 1.9×108 and 2.8×106 fibers per second (f/s), while no free aerosol fibers were detected from sanding Panels A and B containing no CNTs. These free CNT fibers may be a health concern. However, the analysis of particle and EC concentrations from these same samples cannot clearly indicate the presence of CNTs, because extraneous aerosol generation from machining the composite epoxy material increased the mass concentrations of the EC. PMID:26478716

Creating high yield water soluble luminescent graphene quantum dots via exfoliating and disintegrating carbon nanotubes and graphite flakes.

PubMed

Lin, Liangxu; Zhang, Shaowei

2012-10-21

We have developed an effective method to exfoliate and disintegrate multi-walled carbon nanotubes and graphite flakes. With this technique, high yield production of luminescent graphene quantum dots with high quantum yield and low oxidization can be achieved.

75 FR 81349 - Change to the Reporting Date for Certain Data Elements Required Under the Mandatory Reporting of...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-12-27

... steel mills, steel companies, sinter plants, blast furnaces, basic oxygen process furnace shops. Lead... data or data that are less expensive to collect such as process data or material consumption data. For...)(1) Only annual anode consumption (No CEMS). F 98.66(f)(1) Only annual paste consumption (No CEMS). F...

Aluminum for bonding Si-Ge alloys to graphite

DOEpatents

Eggemann, Robert V.

1976-01-13

Improved thermoelectric device and process, comprising the high-temperature, vacuum bonding of a graphite contact and silicon-germanium thermoelectric element by the use of a low void, aluminum, metallurgical shim with low electrical resistance sandwiched therebetween.

Flameless atomic-absorption determination of gold in geological materials

USGS Publications Warehouse

Meier, A.L.

1980-01-01

Gold in geologic material is dissolved using a solution of hydrobromic acid and bromine, extracted with methyl isobutyl ketone, and determined using an atomic-absorption spectrophotometer equipped with a graphite furnace atomizer. A comparison of results obtained by this flameless atomic-absorption method on U.S. Geological Survey reference rocks and geochemical samples with reported values and with results obtained by flame atomic-absorption shows that reasonable accuracy is achieved with improved precision. The sensitivity, accuracy, and precision of the method allows acquisition of data on the distribution of gold at or below its crustal abundance. ?? 1980.

Process for producing metal compounds from graphite oxide

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh (Inventor)

2000-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen This intermediary product can be flier processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Process for Producing Metal Compounds from Graphite Oxide

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh (Inventor)

2000-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon. metal. chloride. and oxygen This intermediary product can be flier processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon. metal carbonate. and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide: b) in an inert environment to produce metal oxide on carbon substrate: c) in a reducing environment. to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Damage tolerance in filament-wound graphite/epoxy pressure vessels

NASA Technical Reports Server (NTRS)

Simon, William E.; Ngueyen, Vinh D.; Chenna, Ravi K.

1995-01-01

Graphite/epoxy composites are extensively used in the aerospace and sporting goods industries due to their superior engineering properties compared to those of metals. However, graphite/epoxy is extremely susceptible to impact damage which can cause considerable and sometimes undetected reduction in strength. An inelastic impact model was developed to predict damage due to low-velocity impact. A transient dynamic finite element formulation was used in conjunction with the 3D Tsai-Wu failure criterion to determine and incorporate failure in the materials during impact. Material degradation can be adjusted from no degradation to partial degradation to full degradation. The developed software is based on an object-oriented implementation framework called Extensible Implementation Framework for Finite Elements (EIFFE).

The Determination of Trace Metals in Saline Waters and Biological Tissues Using the Heated Graphite Atomizer

NASA Technical Reports Server (NTRS)

Segar, D. A.

1971-01-01

A selective, volatalization technique utilizing the heated graphite atomizer atomic absorption technique has been developed for the analysis of iron in sea water. A similar technique may be used to determine vanadium, copper, nickel and cobalt in saline waters when their concentrations are higher than those normally encountered'in unpolluted sea waters. A preliminary solvent extraction using ammonium pyrolidine dithiocarbamate and methyl iso-butyl ketone permits the determination of a number of elements including iron, copper, zinc, nickel, cobalt and lead in sea water. The heated graphite atomized technique has also been applied to the determination of a range of trace transition elements in marine plant and animal tissues.

Cupola Furnace Computer Process Model

DOE Office of Scientific and Technical Information (OSTI.GOV)

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 alloymore » 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).« less

TUBE SPLITTING APPARATUS

DOEpatents

Frantz, C.E.; Cawley, W.E.

1961-05-01

A tool is described for cutting a coolant tube adapted to contain fuel elements to enable the tube to be removed from a graphite moderator mass. The tool splits the tube longitudinally into halves and curls the longitudinal edges of the halves inwardly so that they occupy less space and can be moved radially inwardly away from the walls of the hole in the graphite for easy removal from the graphite.

New Occurrence of Shocked Graphite Aggregates at Barringer Crater

NASA Astrophysics Data System (ADS)

Miura, Y.; Noma, Y.; Iancu, O. G.

1993-07-01

High-pressure carbon minera]s are considered to be formed by solid-solid transformation under static or impact high-pressure condition, but shocked quartz aggregates of impact craters are considered to be formed by quenched accretion of various aggregates by dynamic impact process [1-3]. The main purpose of this study is to elucidate new findings and occurrences of shocked graphite (SG) aggregates [2,3] at the Barringer meteorite crater. The graphite nodule block of Barringer Crater used in this study is collected near the rim. The sample is compared with standard graphite samples of Korea, Madagascar, and artificial impact graphites. There are four different mineral aggregates of the Barringer graphite nodule sample: (1) shocked graphite-1, (2) shocked graphite-2 and hexagonal diamond in the vein, (3) shocked quartz-1 (with kamacite) in the rim, and (4) calcite in the rim (Table 1). X-ray diffraction peaks of shocked graphite reveal low X-ray intensity, high Bragg-angle shift of X-ray diffraction peak, and multiple splitting of X-ray diffraction peaks. X-ray calculated density (rho) has been determined by X-ray diffractometer by the equation of density deviation Delta rho (%) = 100 x {(rho-rho(sub)0)/rho(sub)0}, where standard density rho(sub)0 is 2.255 g/cm^3 in Korean graphite [2,3]. The high-density value of shocked graphite grain obtained in Barringer is Delta rho = +0.6 +/- 0.1%. Shocked hexagonal diamonds (chaoite) show a high value of Delta rho = +0.6 +/- 0.9%. Analytical electron microscopy data reveal three different aggregates in the graphite nodule samples (Table 1): (1) shocked graphite-1 in the matrix, which contains uniformly Fe and Ca elements formed under gas state; (2) shocked graphite-2 in the vein, where crystallized shocked graphites and hexagonal diamonds are surrounded by kamacite-rich metals formed under gas-melt states of mixed compositions from iron meteorite and target rocks; and (3) shocked quartz-1 and kamacite in the rim, where coexisted elements are supplied from kamacite, sandstone, and limestone. The shocked quartz-1 grains with high density contain Fe and Ca elements that are different from the shocked quartz-2 of pure silica [1] formed at the final stage from the Coconino sandstone. (4) Limestone in the rim is attached from Kaibab limestone. The present shocked graphites with high density are the same as artificial fine-grained shocked graphites (Delta rho = +0.7%). Table 1, which appears here in the hard copy, shows formation stages with two shocked graphites in the Barringer Crater. Formation of shocked aggregates with chemical contamination indicate dynamic accretion processes of quenching and depression at impact. The existence of two shocked graphites indicates the two formation stages of the first gas-state and the second gas-melt states with quenching processes. The origin of carbon in the shocked graphites is considered in this study to be from Kaibab limestone. References: [1] Miura Y. (1991) Shock Waves, 1, 35-41. [2] Miura Y. (1992) Proc. Shock Waves (Japan), 2, 54-57. [3] Miura Y. et al. (1993) Symp. NIPR Antarctic Meteorite (Tokyo), in press. [4] Foote A. E. (1891) Am. J. Sci., 42, 413-417. [5] Hannemann R. E. et al. (1967) Science, 155, 995-997.

Graphite fiber polyimide composites for spherical bearings to 340 C (650 F)

NASA Technical Reports Server (NTRS)

Sliney, H. E.; Johnson, R. L.

1972-01-01

Journal bearings with self-alining spherical elements of graphite-fiber-reinforced-polyimide composites were tested from 24 to 340 C (75 to 650 F) at unit loads up to 3.5 times 10 to the 7th power N/sq m (5000 psi). The journal oscillated in the cylindrical bore of the composite element + or - 15 deg at 1 hertz. Outer races and journals were metal hardened of Rockwell C-32 and finished to 10 to the minus 7th power m. A 45 wt. percent graphite-fiber composite gave low friction (0.08 to 0.13), low wear, and almost no plastic deformation under any of the test conditions. Composites with 15 and 25 wt. percent graphite fiber failed by plastic deformation at 315 C (600 F) and 3.5 times 10 to the 7th power N/sq m (5000 psi). A composite with 60 wt. percent graphite fiber failed by brittle fracture under the same conditions, but had very low friction coefficients (0.05 to 0.10) and may be a good bearing material at lighter loads.

Coupled field-structural analysis of HGTR fuel brick using ABAQUS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohanty, S.; Jain, R.; Majumdar, S.

2012-07-01

High-temperature, gas-cooled reactors (HTGRs) are usually helium-gas cooled, with a graphite core that can operate at reactor outlet temperatures much higher than can conventional light water reactors. In HTGRs, graphite components moderate and reflect neutrons. During reactor operation, high temperature and high irradiation cause damage to the graphite crystal and grains and create other defects. This cumulative structural damage during the reactor lifetime leads to changes in graphite properties, which can alter the ability to support the designed loads. The aim of the present research is to develop a finite-element code using commercially available ABAQUS software for the structural integritymore » analysis of graphite core components under extreme temperature and irradiation conditions. In addition, the Reactor Geometry Generator tool-kit, developed at Argonne National Laboratory, is used to generate finite-element mesh for complex geometries such as fuel bricks with multiple pin holes and coolant flow channels. This paper presents the proposed concept and discusses results of stress analysis simulations of a fuel block with H-451 grade material properties. (authors)« less

Comparative inhalation toxicity of multi-wall carbon nanotubes, graphene, graphite nanoplatelets and low surface carbon black.

PubMed

Ma-Hock, Lan; Strauss, Volker; Treumann, Silke; Küttler, Karin; Wohlleben, Wendel; Hofmann, Thomas; Gröters, Sibylle; Wiench, Karin; van Ravenzwaay, Bennard; Landsiedel, Robert

2013-06-17

Carbon nanotubes, graphene, graphite nanoplatelets and carbon black are seemingly chemically identical carbon-based nano-materials with broad technological applications. Carbon nanotubes and carbon black possess different inhalation toxicities, whereas little is known about graphene and graphite nanoplatelets. In order to compare the inhalation toxicity of the mentioned carbon-based nanomaterials, male Wistar rats were exposed head-nose to atmospheres of the respective materials for 6 hours per day on 5 consecutive days. Target concentrations were 0.1, 0.5, or 2.5 mg/m3 for multi-wall carbon nanotubes and 0.5, 2.5, or 10 mg/m3 for graphene, graphite nanoplatelets and low-surface carbon black. Toxicity was determined after end of exposure and after three-week recovery using broncho-alveolar lavage fluid and microscopic examinations of the entire respiratory tract. No adverse effects were observed after inhalation exposure to 10 mg/m3 graphite nanoplatelets or relatively low specific surface area carbon black. Increases of lavage markers indicative for inflammatory processes started at exposure concentration of 0.5 mg/m3 for multi-wall carbon nanotubes and 10 mg/m3 for graphene. Consistent with the changes in lavage fluid, microgranulomas were observed at 2.5 mg/m3 multi-wall carbon nanotubes and 10 mg/m3 graphene. In order to evaluate volumetric loading of the lung as the key parameter driving the toxicity, deposited particle volume was calculated, taking into account different methods to determine the agglomerate density. However, the calculated volumetric load did not correlate to the toxicity, nor did the particle surface burden of the lung. The inhalation toxicity of the investigated carbon-based materials is likely to be a complex interaction of several parameters. Until the properties which govern the toxicity are identified, testing by short-term inhalation is the best option to identify hazardous properties in order to avoid unsafe applications or select safer alternatives for a given application.

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.

Implementation of a numerical holding furnace model in foundry and construction of a reduced model

NASA Astrophysics Data System (ADS)

Loussouarn, Thomas; Maillet, Denis; Remy, Benjamin; Dan, Diane

2016-09-01

Vacuum holding induction furnaces are used for the manufacturing of turbine blades by loss wax foundry process. The control of solidification parameters is a key factor for the manufacturing of these parts in according to geometrical and structural expectations. The definition of a reduced heat transfer model with experimental identification through an estimation of its parameters is required here. In a further stage this model will be used to characterize heat exchanges using internal sensors through inverse techniques to optimize the furnace command and the optimization of its design. Here, an axisymmetric furnace and its load have been numerically modelled using FlexPDE, a finite elements code. A detailed model allows the calculation of the internal induction heat source as well as transient radiative transfer inside the furnace. A reduced lumped body model has been defined to represent the numerical furnace. The model reduction and the estimation of the parameters of the lumped body have been made using a Levenberg-Marquardt least squares minimization algorithm with Matlab, using two synthetic temperature signals with a further validation test.

Inexpensive system protects megawatt resistance-heating furnace against high-voltage surges

NASA Technical Reports Server (NTRS)

Stearns, E. J.

1971-01-01

Coolant gas extinguishes arcing across the break in a heater element. Air-gap shunt which bypasses high voltage impressed across the circuit prevents damage if the resistance elements break and open the inductive circuit.

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

NASA Astrophysics Data System (ADS)

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

2010-09-01

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

Laser excited atomic fluorescence spectrometry as a powerful tool for analytical applications and spectroscopic studies

NASA Astrophysics Data System (ADS)

Gornushkin, Igor B.

1997-12-01

Laser-excited atomic fluorescence spectrometry (LEAFS) with a novel diffusive tube electrothermal atomizer (ETA) has been used for the study of atomization and diffusion processes and for the direct trace analysis of complex matrices. A novel ETA was a graphite tube sealed by two graphite electrodes. A sample was introduced into the tube and the furnace assembly was heated. The vaporized sample diffused through the hot graphite and the atomic fraction of the vapor was excited by a tunable dye laser above the tube. Temporal behavior of atomic fluorescence of Cu, Ag, and Ni atoms, diffused through the furnace tube, was studied at different temperatures; the values for activation energies and diffusion coefficients were derived on the basis of the diffusion/vaporization kinetic model. The femtogram/nanogram concentrations of silver were determined in coastal Atlantic water and soil samples. Use of the new ETA resulted in significant reduction of matrix interferences, ultra-low limits of detection, good accuracy and precision. LEAFS coupled with laser ablation (LA) was studied in terms of its analytical and spectroscopic potential. Low concentrations of lead (0.15 ppm-750 ppm) in metallic matrices (copper, brass, steel, and zinc) were measured in a low pressure argon atmosphere. No matrix effect was observed, providing a universal calibration curve for all samples. A limit of detection of 22 ppb (0.5 fg) was achieved. Also, the lifetime of the metastable 6p21D level of lead was measured and found to be in good agreement with the literature data. A simple open-air LA-LEAFS system was used for the determination of cobalt in solid matrices (graphite, soil, and steel). The fluorescence of cobalt was excited from a level which was already populated in the ablation plasma and was monitored at the Stokes-shifted wavelength. Detection limits in the ppb to ppm range and linearity over four orders of magnitude were achieved. The resonance shadowgraph technique has been developed for time-resolved imaging of laser-produced plasmas. The shadowgraphs were obtained by igniting the plasma on the lead or tin surface and by illuminating the plasma by a laser tuned in resonance with a strong atomic transition. UV-photodecomposition of lead and tin clusters was visualized. The evolution of the plasmas was studied at different pressures of argon. A shock wave produced by the laser ablation was monitored and its speed was measured.

Internal Grains Within KFC Graphites: Implications for Their Stellar Source

NASA Astrophysics Data System (ADS)

Croat, T. K.; Stadermann, F. J.; Bernatowicz, T. J.

2005-03-01

TEM and NanoSIMS investigations find high s-process element enrichments in internal carbides, suggesting an AGB origin for most Murchison KFC presolar graphites. Other rare phases (iron phases and metallic osmium) are consistent with a SN origin.

Spatial clustering of toxic trace elements in adolescents around the Torreón, Mexico lead-zinc smelter.

PubMed

Garcia-Vargas, Gonzalo G; Rothenberg, Stephen J; Silbergeld, Ellen K; Weaver, Virginia; Zamoiski, Rachel; Resnick, Carol; Rubio-Andrade, Marisela; Parsons, Patrick J; Steuerwald, Amy J; Navas-Acién, Ana; Guallar, Eliseo

2014-11-01

High blood lead (BPb) levels in children and elevated soil and dust arsenic, cadmium, and lead were previously found in Torreón, northern Mexico, host to the world's fourth largest lead-zinc metal smelter. The objectives of this study were to determine spatial distributions of adolescents with higher BPb and creatinine-corrected urine total arsenic, cadmium, molybdenum, thallium, and uranium around the smelter. Cross-sectional study of 512 male and female subjects 12-15 years of age was conducted. We measured BPb by graphite furnace atomic absorption spectrometry and urine trace elements by inductively coupled plasma-mass spectrometry, with dynamic reaction cell mode for arsenic. We constructed multiple regression models including sociodemographic variables and adjusted for subject residence spatial correlation with spatial lag or error terms. We applied local indicators of spatial association statistics to model residuals to identify hot spots of significant spatial clusters of subjects with higher trace elements. We found spatial clusters of subjects with elevated BPb (range 3.6-14.7 μg/dl) and urine cadmium (0.18-1.14 μg/g creatinine) adjacent to and downwind of the smelter and elevated urine thallium (0.28-0.93 μg/g creatinine) and uranium (0.07-0.13 μg/g creatinine) near ore transport routes, former waste, and industrial discharge sites. The conclusion derived from this study was that spatial clustering of adolescents with high BPb and urine cadmium adjacent to and downwind of the smelter and residual waste pile, areas identified over a decade ago with high lead and cadmium in soil and dust, suggests that past and/or present plant operations continue to present health risks to children in those neighborhoods.

Feasibility of Rare Earth Element Determination in Low Concentration in Crude Oil: Direct Sampling Electrothermal Vaporization-Inductively Coupled Plasma Mass Spectrometry.

PubMed

Silva, Jussiane Souza; Schneider Henn, Alessandra; Dressler, Valderi Luiz; Mello, Paola Azevedo; Flores, Erico Marlon Moraes

2018-06-05

A comprehensive study was developed showing the feasibility of determination of rare earth elements (REE) in low concentration in crude oil by using direct sampling electrothermal vaporization system coupled to inductively coupled plasma mass spectrometry (ETV-ICP-MS). The effect of organic modifier on the REE signal was evaluated and the use of 6 mg of citric acid allowed calibration using aqueous reference solutions (selected pyrolysis and vaporization temperatures were 700 and 2200 °C, respectively). Because of the facility of REE in forming refractory compounds inside the graphite furnace during the heating step, the use of a modifier gas (Freon R-12, 3.0 mL min -1 ) was necessary to allow quantitative vaporization of these elements. A flow rate of 0.40 L min -1 was selected for both bypass and carrier gases. Under optimized conditions, the influence of sample mass was evaluated, and even using a relatively high mass of crude oil (up to 18 mg), accurate results were obtained. The accuracy was evaluated by the comparison of results by ETV-ICP-MS with those obtained by ICP-MS with ultrasonic nebulizer (USN) after high-pressure microwave-assisted wet digestion (MAWD) and microwave-induced combustion (MIC) and no statistical difference was observed between the results. The limits of quantification for REE by ETV-ICP-MS were lower (0.02-0.8 ng g -1 ) than those obtained by USN-ICP-MS after MAWD and MIC (0.6-5.1 ng g -1 ). Negligible blank values and relative standard deviations lower than 12% show the feasibility of the proposed ETV-ICP-MS method for routine analysis of crude oil.

Spatial clustering of toxic trace elements in adolescents around the Torreón, Mexico lead–zinc smelter

PubMed Central

Garcia-Vargas, Gonzalo G.; Rothenberg, Stephen J.; Silbergeld, Ellen K.; Weaver, Virginia; Zamoiski, Rachel; Resnick, Carol; Rubio-Andrade, Marisela; Parsons, Patrick J.; Steuerwald, Amy J.; Navas-Acién, Ana; Guallar, Eliseo

2016-01-01

High blood lead (BPb) levels in children and elevated soil and dust arsenic, cadmium, and lead were previously found in Torreón, northern Mexico, host to the world’s fourth largest lead–zinc metal smelter. The objectives of this study were to determine spatial distributions of adolescents with higher BPb and creatinine-corrected urine total arsenic, cadmium, molybdenum, thallium, and uranium around the smelter. Cross-sectional study of 512 male and female subjects 12–15 years of age was conducted. We measured BPb by graphite furnace atomic absorption spectrometry and urine trace elements by inductively coupled plasma-mass spectrometry, with dynamic reaction cell mode for arsenic. We constructed multiple regression models including sociodemographic variables and adjusted for subject residence spatial correlation with spatial lag or error terms. We applied local indicators of spatial association statistics to model residuals to identify hot spots of significant spatial clusters of subjects with higher trace elements. We found spatial clusters of subjects with elevated BPb (range 3.6–14.7 µg/dl) and urine cadmium (0.18–1.14 µg/g creatinine) adjacent to and downwind of the smelter and elevated urine thallium (0.28–0.93 µg/g creatinine) and uranium (0.07–0.13 µg/g creatinine) near ore transport routes, former waste, and industrial discharge sites. The conclusion derived from this study was that spatial clustering of adolescents with high BPb and urine cadmium adjacent to and downwind of the smelter and residual waste pile, areas identified over a decade ago with high lead and cadmium in soil and dust, suggests that past and/or present plant operations continue to present health risks to children in those neighborhoods. PMID:24549228

Design considerations regarding an atomizer for multi-element electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Katskov, Dmitri A.; Sadagov, Yuri M.

2011-06-01

The methodology of simultaneous multi-element electrothermal atomic absorption spectrometry (ETAAS-Electrothermal Atomic Absorption Spectrometry) stipulates rigid requirements to the design and operation of the atomizer. It must provide high degree of atomization for the group of analytes, invariant respective to the vaporization kinetics and heating ramp residence time of atoms in the absorption volume and absence of memory effects from major sample components. For the low resolution spectrometer with a continuum radiation source the reduced compared to traditional ETAAS (Electrothermal Atomic Absorption Spectrometry) sensitivity should be, at least partially, compensated by creating high density of atomic vapor in the absorption pulse. The sought-for characteristics were obtained for the 18 mm in length and 2.5 mm in internal diameter longitudinally heated graphite tube atomizer furnished with 2-4.5 mg of ring shaped carbon fiber yarn collector. The collector located next to the sampling port provides large substrate area that helps to keep the sample and its residue in the central part of the tube after drying. The collector also provides a "platform" effect that delays the vaporization and stipulates vapor release into absorption volume having already stabilized gas temperature. Due to the shape of external surface of the tube, presence of collector and rapid (about 10 °C/ms) heating, an inverse temperature distribution along the tube is attained at the beginnings of the atomization and cleaning steps. The effect is employed for cleaning of the atomizer using the set of short maximum power heating pulses. Preparation, optimal maintenance of the atomizer and its compliance to the multi-element determination requirements are evaluated and discussed. The experimental setup provides direct simultaneous determination of large group of element within 3-4 order concentration range. Limits of detection are close to those for sequential single element determination in Flame AAS with primary line source that is 50-1000 times higher than the limits obtainable with common ETAAS (Electrothermal Atomic Absorption Spectrometry) instrumentation.

DOE Office of Scientific and Technical Information (OSTI.GOV)

S. Dong; N. Paterson; S.G. Kazarian

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

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.

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.

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

PubMed

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

2018-03-01

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

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.

A Plenoptic Multi-Color Imaging Pyrometer

NASA Technical Reports Server (NTRS)

Danehy, Paul M.; Hutchins, William D.; Fahringer, Timothy; Thurow, Brian S.

2017-01-01

A three-color pyrometer has been developed based on plenoptic imaging technology. Three bandpass filters placed in front of a camera lens allow separate 2D images to be obtained on a single image sensor at three different and adjustable wavelengths selected by the user. Images were obtained of different black- or grey-bodies including a calibration furnace, a radiation heater, and a luminous sulfur match flame. The images obtained of the calibration furnace and radiation heater were processed to determine 2D temperature distributions. Calibration results in the furnace showed that the instrument can measure temperature with an accuracy and precision of 10 Kelvins between 1100 and 1350 K. Time-resolved 2D temperature measurements of the radiation heater are shown.

A high-temperature furnace for in situ synchrotron X-ray spectroscopy under controlled atmospheric conditions.

PubMed

Eeckhout, Sigrid Griet; Gorges, Bernard; Barthe, Laurent; Pelosi, Orietta; Safonova, Olga; Giuli, Gabriele

2008-09-01

A high-temperature furnace with an induction heater coil has been designed and constructed for in situ X-ray spectroscopic experiments under controlled atmospheric conditions and temperatures up to 3275 K. The multi-purpose chamber design allows working in backscattering and normal fluorescence mode for synchrotron X-ray absorption and emission spectroscopy. The use of the furnace is demonstrated in a study of the in situ formation of Cr oxide between 1823 K and 2023 K at logPO(2) values between -10.0 and -11.3 using X-ray absorption near-edge spectroscopy. The set-up is of particular interest for studying liquid metals, alloys and other electrically conductive materials under extreme conditions.

Concentrating Solar Power Projects - Lake Cargelligo | Concentrating Solar

Science.gov Websites

Solar Storage Receiver, set out in a multi tower solar array. The Project consists of eight SSR's each mounted on its own tower. This graphite receiver acts as receiver, boiler and storage system. Status Date Manufacturer: Lloyd Energy Systems Pty Ltd Receiver Type: Graphite solar storage receiver Heat-Transfer Fluid

Advanced Ceramics for Use as Fuel Element Materials in Nuclear Thermal Propulsion Systems

NASA Technical Reports Server (NTRS)

Valentine, Peter G.; Allen, Lee R.; Shapiro, Alan P.

2012-01-01

With the recent start (October 2011) of the joint National Aeronautics and Space Administration (NASA) and Department of Energy (DOE) Advanced Exploration Systems (AES) Nuclear Cryogenic Propulsion Stage (NCPS) Program, there is renewed interest in developing advanced ceramics for use as fuel element materials in nuclear thermal propulsion (NTP) systems. Three classes of fuel element materials are being considered under the NCPS Program: (a) graphite composites - consisting of coated graphite elements containing uranium carbide (or mixed carbide), (b) cermets (ceramic/metallic composites) - consisting of refractory metal elements containing uranium oxide, and (c) advanced carbides consisting of ceramic elements fabricated from uranium carbide and one or more refractory metal carbides [1]. The current development effort aims to advance the technology originally developed and demonstrated under Project Rover (1955-1973) for the NERVA (Nuclear Engine for Rocket Vehicle Application) [2].

Trace elements in sera of patients with hepatitis B: Determination and analysis

NASA Astrophysics Data System (ADS)

Saod, Wahran M.; Darwish, Nadiya T.; Zaidan, Tahseen A.; Alfalujie, Abdul Wahab A.

2018-04-01

Chronic Hepatitis B (HBV) is the leading cause of morbidity and mortality worldwide with about 248 million people having HBV infection. Trace elements e.g. copper (Cu), zinc (Zn), selenium (Se) and iron (Fe) are constituent components of many metal proteins and metalloenzymes in human sera. Therefore, the ratios of these trace elements in human sera are often stated to be a good marker for diagnosing various diseases including HBV. The aims of this study are: to compare the level of trace elements in sera of patients infected with HBV and healthy participants, and to evaluate the efficiency of analytical techniques (e.g. Inductively Coupled Plasma-Mass spectrometry (ICP-MS), Atomic Absorption Spectroscopy (hydride generation) (AAS) and Graphite Furnace Atomic Absorption Spectroscopy (GFAAS) that are currently used to detect Fe and Se elements in Patients' human sera. The findings of this study show that the concentration range of copper element between (132.80±28.64 µg/dl) to (105.66±23.20 µg/dl) was significantly higher in HBV infected patients as compared to those in healthy controls (91.27±9.20 µg/dl). Iron concentration range between (206.64±61.60 µg/l) to (170.00±36.71 µg/l) was significantly higher in HBV infected patients as compared to those in healthy controls (158.00±15.13 µg/l). However, patients with HBV had significantly lower serum concentrations of zinc with a concentration range between (111.64±20.90 µg/dl) to (99.25±24.06 µg/dl) as compared to those in healthy controls (113.44±16.38 µg/dl). While selenium concentration range between (64.39±7.39 µg/l) to (51.10±4.96 µg/l) was significantly lower in HBV infected patients as compared to those in healthy controls (67.68±7.60) (μg/l). Moreover, the results of this study suggest that (AAS) technique was the most accurate method to measure the concentration of selenium element, while (UV and ICP-MS) analytical techniques have the same efficiency in measuring the iron concentration.

Method for starting operation of a resistance melter

DOEpatents

Chapman, Christopher Charles

1977-01-01

A method for starting the operation of a resistance furnace, where heating occurs by passing a current through the charge between two furnace electrodes and the charge is a material which is essentially electrically nonconductive when in a solid physical state but which becomes more electrically conductive when in a molten physical state, by connecting electrical resistance heating wire between the furnace electrodes, placing the wire in contact with the charge material between the electrodes and passing a current through the wire to heat the wire to a temperature sufficient to melt the material between the furnace electrodes so that as the material melts, current begins to pass between the electrodes through the melted material, further heating and melting more material until all current between the electrodes passes through the charge material without the aid or presence of the resistance element.

Paired Straight Hearth Furnace - Transformational Ironmaking Process

DOE Office of Scientific and Technical Information (OSTI.GOV)

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 suitablemore » 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.« less

Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples.

PubMed

Boulyga, Sergei F; Heilmann, Jens; Prohaska, Thomas; Heumann, Klaus G

2007-10-01

A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for (35)Cl+ to more than 6 x 10(5) cps for (238)U+ for 1 microg of trace element per gram of coal sample. Detection limits vary from 450 ng g(-1) for chlorine and 18 ng g(-1) for sulfur to 9.5 pg g(-1) for mercury and 0.3 pg g(-1) for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis.

FUEL ELEMENT FOR A NUCLEAR REACTOR

DOEpatents

Davidson, J.K.

1963-11-19

A fuel element structure particularly useful in high temperature nuclear reactors is presented. Basically, the structure comprises two coaxial graphite sleeves integrally joined together by radial fins. Due to the high structural strength of graphite at high temperatures and the rigidity of this structure, nuclear fuel encased within the inner sleeve in contiguous relation therewith is supported and prevented from expanding radially at high temperatures. Thus, the necessity of relying on the usual cladding materials with relatively low temperature limitations for structural strength is removed. (AEC)

Multi-ampoule Bridgman growth of halide scintillator crystals using the self-seeding method

NASA Astrophysics Data System (ADS)

Lindsey, Adam C.; Wu, Yuntao; Zhuravleva, Mariya; Loyd, Matthew; Koschan, Merry; Melcher, Charles L.

2017-07-01

We investigate the multi-ampoule growth at 25 mm diameter of ternary iodide single crystal scintillator KCaI3:Eu using the randomly oriented self-seeded Bridgman method. We compare scintillation performance between cubic inch scale crystals containing small variations of low nominal europium concentrations previously shown to balance light yield with self-absorption in the host crystal. Growth conditions were optimized in the developmental furnace and four 2 in3 KCaI3:Eu crystals were grown simultaneously producing a total of six 25 mm × 25 mm cylinders. Small variations in activator concentration did not result in significant performance differences among the six measured crystals. A range of energy resolutions of 3.5-4.7% at 662 keV was achieved, surpassing that of NaI:Tl crystals commonly used in spectroscopic detection applications. The function and basic design of the multi-ampoule furnace as well as the process of growing single crystals of KCaI3 is included here.

They Came from the Deep in the Supernova: The Origin of TiC and Metal Subgrains in Presolar Graphite Grains

NASA Astrophysics Data System (ADS)

Lodders, Katharina

2006-08-01

A new formation scenario for TiC and Fe-Ni metal inclusions in presolar graphite grains of supernova origin is described. The mineralogy and chemistry require condensation of Fe-Ni titanides from Fe-, Ni-, and Ti-rich gaseous ejecta, subsequent carburization to make TiC and metal, and encapsulation into graphite. Titanides only condense if Si is depleted relative to heavier elements, which requires α-rich freeze-out and a deep mass cut for the supernova ejecta. This Si-poor core material must remain unmixed with other supernova zones until the titanides condense. This can be accomplished by transport of core ejecta in bipolar jets through the major expanding supernova zone ejecta. If the jets stall in regions dominated by C-rich ejecta such as the C-He zone, where graphite condenses, thermochemically favored in situ carburization of the titanides-either before or during encapsulation into condensing graphite-leads to a TiC-and-metal composite. This scenario agrees with theoretical models and observations of asymmetric core collapse in supernovae that are associated with bipolar jets loaded with iron-peak elements.

Three-Dimensional Imaging and Numerical Reconstruction of Graphite/Epoxy Composite Microstructure Based on Ultra-High Resolution X-Ray Computed Tomography

NASA Technical Reports Server (NTRS)

Czabaj, M. W.; Riccio, M. L.; Whitacre, W. W.

2014-01-01

A combined experimental and computational study aimed at high-resolution 3D imaging, visualization, and numerical reconstruction of fiber-reinforced polymer microstructures at the fiber length scale is presented. To this end, a sample of graphite/epoxy composite was imaged at sub-micron resolution using a 3D X-ray computed tomography microscope. Next, a novel segmentation algorithm was developed, based on concepts adopted from computer vision and multi-target tracking, to detect and estimate, with high accuracy, the position of individual fibers in a volume of the imaged composite. In the current implementation, the segmentation algorithm was based on Global Nearest Neighbor data-association architecture, a Kalman filter estimator, and several novel algorithms for virtualfiber stitching, smoothing, and overlap removal. The segmentation algorithm was used on a sub-volume of the imaged composite, detecting 508 individual fibers. The segmentation data were qualitatively compared to the tomographic data, demonstrating high accuracy of the numerical reconstruction. Moreover, the data were used to quantify a) the relative distribution of individual-fiber cross sections within the imaged sub-volume, and b) the local fiber misorientation relative to the global fiber axis. Finally, the segmentation data were converted using commercially available finite element (FE) software to generate a detailed FE mesh of the composite volume. The methodology described herein demonstrates the feasibility of realizing an FE-based, virtual-testing framework for graphite/fiber composites at the constituent level.

Study of evaporating the irradiated graphite in equilibrium low-temperature plasma

NASA Astrophysics Data System (ADS)

Bespala, E. V.; Novoselov, I. Yu.; Pavlyuk, A. O.; Kotlyarevskiy, S. G.

2018-01-01

The paper describes a problem of accumulation of irradiated graphite due to operation of uranium-graphite nuclear reactors. The main noncarbon contaminants that contribute to the overall activity of graphite elements are iso-topes 137Cs, 60Co, 90Sr, 36Cl, and 3H. A method was developed for processing of irradiated graphite ensuring the volu-metric decontamination of samples. The calculation results are presented for equilibrium composition of plasma-chemical reactions in systems "irradiated graphite-argon" and "irradiated graphite-helium" for a wide range of tem-peratures. The paper describes a developed mathematical model for the process of purification of a porous graphite surface treated by equilibrium low-temperature plasma. The simulation results are presented for the rate of sublimation of radioactive contaminants as a function of plasma temperature and plasma flow velocity when different plasma-forming gases are used. The extraction coefficient for the contaminant 137Cs from the outer side of graphite pores was calculated. The calculations demonstrated the advantages of using a lighter plasma forming gas, i.e., helium.

High Temperature Mechanical Characterization of Ceramic Matrix Composites

NASA Technical Reports Server (NTRS)

Gyekenyesi, John Z.

1998-01-01

A high temperature mechanical characterization laboratory has been assembled at NASA Lewis Research Center. One contribution of this work is to test ceramic matrix composite specimens in tension in environmental extremes. Two high temperature tensile testing systems were assembled. The systems were assembled based on the performance and experience of other laboratories and meeting projected service conditions for the materials in question. The systems use frames with an electric actuator and a center screw. A PC based data acquisition and analysis system is used to collect and analyze the data. Mechanical extensometers are used to measure specimen strain. Thermocouples, placed near the specimen, are used to measure the specimen gage section temperature. The system for testing in air has a resistance element furnace with molybdenum disilicide elements and pneumatic grips with water cooling attached to hydraulic alignment devices. The system for testing in an inert gas has a graphite resistance element furnace in a chamber with rigidly mounted, water cooled, hydraulically actuated grips. Unidirectional SiC fiber reinforced reaction bonded Si3N4 and triaxially woven, two dimensional, SiC fiber reinforced enhanced SiC composites were tested in unidirectional tension. Theories for predicting the Young's modulus, modulus near the ultimate strength, first matrix cracking stress, and ultimate strength were applied and evaluated for suitability in predicting the mechanical behavior of SiC/RBSN and enhanced SiC/SiC composites. The SiC/RBSN composite exhibited pseudo tough behavior (increased area under the stress/strain curve) from 22 C to 1500 C. The rule of mixtures provides a good estimate of the Young's modulus of the SiC/RBSN composite using the constituent properties from room temperature to 1440 C for short term static tensile tests in air or nitrogen. The rule of mixtures significantly overestimates the secondary modulus near the ultimate strength. The ACK theory provides the best approximation of the first matrix cracking stress when residual stresses are ignored. The theory of Cao and Thouless, based on Weibull statistics, gave the best prediction for the composite ultimate strength. The enhanced SiC/SiC composite exhibited nonlinear stress/strain behavior from 24 C to 1370 C in air with increased ultimate strain when compared to monolithic SiC. The theory of Yang and Chou with the assumption of a frictional fiber/matrix interface provided the best estimate of the Young's modulus. The theory of Cao and Thouless gave the best estimate for the ultimate strength.

Multidisciplinary Simulation of Graphite-Composite and Cermet Fuel Elements for NTP Point of Departure Designs

NASA Technical Reports Server (NTRS)

Stewart, Mark E.; Schnitzler, Bruce G.

2015-01-01

This paper compares the expected performance of two Nuclear Thermal Propulsion fuel types. High fidelity, fluid/thermal/structural + neutronic simulations help predict the performance of graphite-composite and cermet fuel types from point of departure engine designs from the Nuclear Thermal Propulsion project. Materials and nuclear reactivity issues are reviewed for each fuel type. Thermal/structural simulations predict thermal stresses in the fuel and thermal expansion mis-match stresses in the coatings. Fluid/thermal/structural/neutronic simulations provide predictions for full fuel elements. Although NTP engines will utilize many existing chemical engine components and technologies, nuclear fuel elements are a less developed engine component and introduce design uncertainty. Consequently, these fuel element simulations provide important insights into NTP engine performance.

Nonlinear static and dynamic finite element analysis of an eccentrically loaded graphite-epoxy beam

NASA Technical Reports Server (NTRS)

Fasanella, Edwin L.; Jackson, Karen E.; Jones, Lisa E.

1991-01-01

The Dynamic Crash Analysis of Structures (DYCAT) and NIKE3D nonlinear finite element codes were used to model the static and implulsive response of an eccentrically loaded graphite-epoxy beam. A 48-ply unidirectional composite beam was tested under an eccentric axial compressive load until failure. This loading configuration was chosen to highlight the capabilities of two finite element codes for modeling a highly nonlinear, large deflection structural problem which has an exact solution. These codes are currently used to perform dynamic analyses of aircraft structures under impact loads to study crashworthiness and energy absorbing capabilities. Both beam and plate element models were developed to compare with the experimental data using the DYCAST and NIKE3D codes.

Auger electron and X-ray photoelectron spectroscopic study of the biocorrosion of copper by alginic acid polysaccharide

NASA Astrophysics Data System (ADS)

Jolley, John G.; Geesey, Gill G.; Hankins, Michael R.; Wright, Randy B.; Wichlacz, Paul L.

1989-08-01

Thin films (3.4 nm) of copper on germanium substrates were exposed to 2% alginic acid polysaccharide aqueous solution. Pre- and post-exposure characterization were done by Auger electron spectroscopy and X-ray photoelectron spectroscopy. Ancillary graphite furnace atomic absorption spectroscopy was used to monitor the removal process of the copper thin film from the germanium substrate. Results indicate that some of the copper was oxidized by the alginic acid solution. Some of the copper was removed from the Cu/Ge interface and incorporated into the polymer matrix. Thus, biocorrosion of copper was exhibited by the alginic acid polysaccharide.

FTIR Monitoring Of Curing Of Composites

NASA Technical Reports Server (NTRS)

Druy, Mark A.; Stevenson, William A.; Young, Philip R.

1990-01-01

Infrared-sensing optical fiber system developed to monitor principal infrared absorption bands resulting from vibrations of atoms and molecules as chemical bonds form when resin cured. System monitors resin chemistry more directly. Used to obtain Fourier transform infrared (FTIR) spectrum from graphite fiber/polyimide matrix resin prepreg. Embedded fiber optic FTIR sensor used to indicate state of cure of thermosetting composite material. Developed primarily to improve quality of advanced composites, many additional potential applications exist because principal of operation applicable to all organic materials and most inorganic gases. Includes monitoring integrities of composite materials in service, remote sensing of hazardous materials, and examination of processes in industrial reactors and furnaces.

Dispersion toughened ceramic composites and method for making same

DOEpatents

Stinton, David P.; Lackey, Walter J.; Lauf, Robert J.

1986-01-01

Ceramic composites exhibiting increased fracture toughness are produced by the simultaneous codeposition of silicon carbide and titanium disilicide by chemical vapor deposition. A mixture of hydrogen, methyltrichlorosilane and titanium tetrachloride is introduced into a furnace containing a substrate such as graphite or silicon carbide. The thermal decomposition of the methyltrichlorosilane provides a silicon carbide matrix phase and the decomposition of the titanium tetrachloride provides a uniformly dispersed second phase of the intermetallic titanium disilicide within the matrix phase. The fracture toughness of the ceramic composite is in the range of about 6.5 to 7.0 MPa.sqroot.m which represents a significant increase over that of silicon carbide.

Dispersion toughened ceramic composites and method for making same

DOEpatents

Stinton, D.P.; Lackey, W.J.; Lauf, R.J.

1984-09-28

Ceramic composites exhibiting increased fracture toughness are produced by the simultaneous codeposition of silicon carbide and titanium disilicide by chemical vapor deposition. A mixture of hydrogen, methyltrichlorosilane and titanium tetrachloride is introduced into a furnace containing a substrate such as graphite or silicon carbide. The thermal decomposition of the methyltrichlorosilane provides a silicon carbide matrix phase and the decomposition of the titanium tetrachloride provides a uniformly dispersed second phase of the intermetallic titanium disilicide within the matrix phase. The fracture toughness of the ceramic composite is in the range of about 6.5 to 7.0 MPa..sqrt..m which represents a significant increase over that of silicon carbide.

Comparative in vitro biocompatibility of nickel-titanium, pure nickel, pure titanium, and stainless steel: genotoxicity and atomic absorption evaluation.

PubMed

Assad, M; Lemieux, N; Rivard, C H; Yahia, L H

1999-01-01

The genotoxicity level of nickel-titanium (NiTi) was compared to that of its pure constituents, pure nickel (Ni) and pure titanium (Ti) powders, and also to 316L stainless steel (316L SS) as clinical reference material. In order to do so, a dynamic in vitro semiphysiological extraction was performed with all metals using agitation and ISO requirements. Peripheral blood lymphocytes were then cultured in the presence of all material extracts, and their comparative genotoxicity levels were assessed using electron microscopy-in situ end-labeling (EM-ISEL) coupled to immunogold staining. Cellular chromatin exposition to pure Ni and 316L SS demonstrated a significantly stronger gold binding than exposition to NiTi, pure Ti, or the untreated control. In parallel, graphite furnace atomic absorption spectrophotometry (AAS) was also performed on all extraction media. The release of Ni atoms took the following decreasing distribution for the different resulting semiphysiological solutions: pure Ni, 316L SS, NiTi, Ti, and controls. Ti elements were detected after elution of pure titanium only. Both pure titanium and nickel-titanium specimens obtained a relative in vitro biocompatibility. Therefore, this quantitative in vitro study provides optimistic results for the eventual use of nickel-titanium alloys as surgical implant materials.

Systemic levels of metallic ions released from orthodontic mini-implants.

PubMed

de Morais, Liliane Siqueira; Serra, Glaucio Guimarães; Albuquerque Palermo, Elisabete Fernandes; Andrade, Leonardo Rodrigues; Müller, Carlos Alberto; Meyers, Marc André; Elias, Carlos Nelson

2009-04-01

Orthodontic mini-implants are a potential source of metallic ions to the human body because of the corrosion of titanium (Ti) alloy in body fluids. The purpose of this study was to gauge the concentration of Ti, aluminum (Al), and vanadium (V), as a function of time, in the kidneys, livers, and lungs of rabbits that had Ti-6Al-4V alloy orthodontic mini-implants placed in their tibia. Twenty-three New Zealand rabbits were randomly divided into 4 groups: control, 1 week, 4 weeks, and 12 weeks. Four orthodontic mini-implants were placed in the left proximal tibia of 18 rabbits. Five control rabbits had no orthodontic mini-implants. After 1, 4, and 12 weeks, the rabbits were killed, and the selected tissues were extracted and prepared for analysis by graphite furnace atomic absorption spectrophotometry. Low amounts of Ti, Al, and V were detectable in the 1-week, 4-weeks, and 12-weeks groups, confirming that release of these metals from the mini-implants occurs, with diffusion and accumulation in remote organs. Despite the tendency of ion release when using the Ti alloy as orthodontic mini-implants, the amounts of metals detected were significantly below the average intake of these elements through food and drink and did not reach toxic concentrations.

Metal release rate from AISI 316L stainless steel and pure Fe, Cr and Ni into a synthetic biological medium--a comparison.

PubMed

Herting, G; Wallinder, I Odnevall; Leygraf, C

2008-09-01

Metal release rates from stainless steel grade 316L were investigated in artificial lysosomal fluid (ALF), simulating a human inflammatory cell response. The main focus was placed on release rates of main alloying elements using graphite furnace atomic absorption spectroscopy, and changes in surface oxide composition by means of X-ray photoelectron spectroscopy. To emphasise that alloys and pure metals possess totally different intrinsic properties, comparative studies were performed on the pure alloying constituents: iron, nickel and chromium. Significant differences in release rates were observed due to the presence of a passive surface film on stainless steel. Iron and nickel were released at rates more than 300 times lower from the 316L alloy compared with the pure metals whereas the release rate of chromium was similar. Iron was preferentially released compared with nickel and chromium. Immersion in ALF resulted in the gradual enrichment of chromium in the surface film, a small increase of nickel, and the reduction of oxidized iron with decreasing release rates of alloy constituents as a result. As expected, released metals from stainless steel grade 316L were neither in proportion to the bulk alloy composition nor to the surface film composition.

Effect of Copper and Silicon on Al-5%Zn Alloy as a Candidate Low Voltage Sacrificial Anode

NASA Astrophysics Data System (ADS)

Pratesa, Yudha; Ferdian, Deni; Togina, Inez

2017-05-01

One common method used for corrosion protection is a sacrificial anode. Sacrificial anodes that usually employed in the marine environment are an aluminum alloy sacrificial anode, especially Al-Zn-In. However, the electronegativity of these alloys can cause corrosion overprotection and stress cracking (SCC) on a high-strength steel. Therefore, there is a development of the sacrificial anode aluminum low voltage to reduce the risk of overprotection. The addition of alloying elements such as Cu, Si, and Ge will minimize the possibility of overprotection. This study was conducted to analyze the effect of silicon and copper addition in Al-5Zn. The experiment started from casting the sacrificial anode aluminum uses electrical resistance furnace in a graphite crucible in 800°C. The results alloy was analyzed using Optical emission spectroscopy (OES), Differential scanning calorimetry, electrochemical impedance spectroscopy, and metallography. Aluminum alloy with the addition of a copper alloy is the most suitable and efficient to serve as a low-voltage sacrificial anode aluminum. Charge transfer resistivity of copper is smaller than silicon which indicates that the charge transfer between the metal and the electrolyte is easier t to occur. Also, the current potential values in coupling with steel are also in the criteria range of low-voltage aluminum sacrificial anodes.

Heterojunction photodiode on cleaved SiC

NASA Astrophysics Data System (ADS)

Solovan, Mykhailo M.; Farah, John; Kovaliuk, Taras T.; Brus, Viktor V.; Mostovyi, Andrii I.; Maistruk, Eduard V.; Maryanchuk, Pavlo D.

2018-01-01

Graphite/n-SiC Shottky diodes were prepared by means of the recently proposed technique based on the transferring of drawn graphite films onto the n-SiC single crystal substrate. Current-voltage characteristics were measured and analyzed. High quality ohmic contancts were prepared by the DC magnetron sputtering of Ni thin films onto cleaved n-type SiC single crystal substrates. The height of the potential barrier and the series resistance of the graphite/n-SiC junctions were measured and analysed. The dominant current transport mechanisms through the diodes were determined. There was shown that the dominant current transport mechanisms through the graphite/n-SiC Shottky diodes were the multi-step tunnel-recombination at forward bias and the tunnelling mechanisms at reverse bias.

Comparative inhalation toxicity of multi-wall carbon nanotubes, graphene, graphite nanoplatelets and low surface carbon black

PubMed Central

2013-01-01

Background Carbon nanotubes, graphene, graphite nanoplatelets and carbon black are seemingly chemically identical carbon-based nano-materials with broad technological applications. Carbon nanotubes and carbon black possess different inhalation toxicities, whereas little is known about graphene and graphite nanoplatelets. Methods In order to compare the inhalation toxicity of the mentioned carbon-based nanomaterials, male Wistar rats were exposed head-nose to atmospheres of the respective materials for 6 hours per day on 5 consecutive days. Target concentrations were 0.1, 0.5, or 2.5 mg/m3 for multi-wall carbon nanotubes and 0.5, 2.5, or 10 mg/m3 for graphene, graphite nanoplatelets and low-surface carbon black. Toxicity was determined after end of exposure and after three-week recovery using broncho-alveolar lavage fluid and microscopic examinations of the entire respiratory tract. Results No adverse effects were observed after inhalation exposure to 10 mg/m3 graphite nanoplatelets or relatively low specific surface area carbon black. Increases of lavage markers indicative for inflammatory processes started at exposure concentration of 0.5 mg/m3 for multi-wall carbon nanotubes and 10 mg/m3 for graphene. Consistent with the changes in lavage fluid, microgranulomas were observed at 2.5 mg/m3 multi-wall carbon nanotubes and 10 mg/m3 graphene. In order to evaluate volumetric loading of the lung as the key parameter driving the toxicity, deposited particle volume was calculated, taking into account different methods to determine the agglomerate density. However, the calculated volumetric load did not correlate to the toxicity, nor did the particle surface burden of the lung. Conclusions The inhalation toxicity of the investigated carbon-based materials is likely to be a complex interaction of several parameters. Until the properties which govern the toxicity are identified, testing by short-term inhalation is the best option to identify hazardous properties in order to avoid unsafe applications or select safer alternatives for a given application. PMID:23773277

Research on the transformation mechanism of graphite phase and microstructure in the heated region of gray cast iron by laser cladding

NASA Astrophysics Data System (ADS)

Liu, Yancong; Zhan, Xianghua; Yi, Peng; Liu, Tuo; Liu, Benliang; Wu, Qiong

2018-03-01

A double-track lap cladding experiment involving gray cast iron was established to investigate the transformation mechanism of graphite phase and microstructure in a laser cladding heated region. The graphite phase and microstructure in different heated regions were observed under a microscope, and the distribution of elements in various heated regions was analyzed using an electron probe. Results show that no graphite existed in the cladding layer and in the middle and upper parts of the binding region. Only some of the undissolved small graphite were observed at the bottom of the binding region. Except the refined graphite size, the morphological characteristics of substrate graphite and graphite in the heat-affected zone were similar. Some eutectic clusters, which grew along the direction of heat flux, were observed in the heat-affected zone whose microstructure was transformed into a mixture of austenite, needle-like martensite, and flake graphite. Needle-like martensite around graphite was fine, but this martensite became sparse and coarse when it was away from graphite. Some martensite clusters appeared in the local area near the binding region, and the carbon atoms in the substrate did not diffuse into the cladding layer through laser cladding, which only affected the bonding area and the bottom of the cladding layer.

Effect of Amount of Carbon on the Reduction Efficiency of Iron Ore-Coal Composite Pellets in Multi-layer Bed Rotary Hearth Furnace (RHF)

NASA Astrophysics Data System (ADS)

Mishra, Srinibash; Roy, Gour Gopal

2016-08-01

The effect of carbon-to-hematite molar ratio has been studied on the reduction efficiency of iron ore-coal composite pellet reduced at 1523 K (1250 °C) for 20 minutes in a laboratory scale multi-layer bed rotary hearth furnace (RHF). Reduced pellets have been characterized through weight loss measurement, estimation of porosity, shrinkage, qualitative and quantitative phase analysis by XRD. Performance parameters such as the degree of reduction, metallization, carbon efficiency, productivity, and compressive strength have been calculated to compare the process efficacy at different carbon levels in the pellets. Pellets with optimum carbon-to-hematite ratio (C/Fe2O3 molar ratio = 1.66) that is much below the stoichiometric carbon required for direct reduction of hematite yielded maximum reduction, better carbon utilization, and productivity for all three layers. Top layer exhibited maximum reduction at comparatively lower carbon level (C/Fe2O3 molar ratio <2.33) in the pellet, while bottom layer exceeded top layer reduction at higher carbon level (C/Fe2O3 molar ratio >2.33). Correlation between degree of reduction and metallization indicated non-isothermal kinetics influenced by heat and mass transfer in multi-layer bed RHF. Compressive strength of the partially reduced pellet with optimum carbon content (C/Fe2O3 molar ratio = 1.66) showed that they could be potentially used as an alternate feed in a blast furnace or any other smelting reactor.

The effect of synthesis time on graphene growth from palm oil as green carbon precursor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Salifairus, M. J., E-mail: salifairus-mj85@yahoo.co.uk; Faculty of Applied Sciences, Universiti Teknologi MARA; NANO-ElecTronic Centre - Faculty of Electrical Engineering, Universiti Teknologi MARA

2016-07-06

Graphene is the new material that arises after carbon nanotubes (CNTs) era and has extraordinary optical, electronic and mechanical properties compared to CNTs. The 2D graphene is the sp{sup 2} carbon allotropes compared to other dimensionality. It also can be in three forms that are zero-dimensional, one-dimensional or three-dimensional. The different dimensionality also called fullerenes, nanotubes and graphite. Therefore, the graphene is known as centre potential materials in expanding research area than others ever. The 2 cm × 2 cm silicon wafer was seeded with nickel (Ni) at different thickness by using sputter coater. The palm oil, carbon source, wasmore » placed in the precursor furnace and the silicon was placed in the second furnace (deposition furnace). The palm oil will mix with Nitrogen gas was used as carrier gas in the CVD under certain temperature and pressure to undergo pyrolysis proses. The deposition temperature was set at 1000 °C. The deposition time varied from 3 minutes, 5 minutes and 7 minutes. The graphene was growth at ambient pressure in the CVD system. Electron microscopy and Raman Spectrometer revealed the structural properties and surface morphology of the grapheme on the substrate. The D and G band appear approximately at 1350 cm{sup −1} and 1850 cm{sup −1}. It can be concluded that the growth of graphene varies at different deposition time.« less

Recycling of aluminium scrap for secondary Al-Si alloys.

PubMed

Velasco, Eulogio; Nino, Jose

2011-07-01

An increasing amount of recycled aluminium is going into the production of aluminium alloy used for automotive applications. In these applications, it is necessary to control and remove alloy impurities and inclusions. Cleaning and fluxing processes are widely used during processing of the alloys for removal of inclusions, hydrogen and excess of magnesium. These processes use salt fluxes based in the system NaCl-KCl, injection of chlorine or mixture of chlorine with an inert gas. The new systems include a graphite wand and a circulation device to force convection in the melt and permit the bubbling and dispersion of reactive and cleaning agents. This paper discusses the recycling of aluminium alloys in rotary and reverberatory industrial furnaces. It focuses on the removal of magnesium during the melting process. In rotary furnaces, the magnesium lost is mainly due to the oxidation process at high temperatures. The magnesium removal is carried out by the reaction between chlorine and magnesium, with its efficiency associated to kinetic factors such as concentration of magnesium, mixing, and temperature. These factors are also related to emissions generated during the demagging process. Improvements in the metallic yield can be reached in rotary furnaces if the process starts with a proper salt, with limits of addition, and avoiding long holding times. To improve throughput in reverberatories, start the charging with high magnesium content material and inject chlorine gas if the molten metal is at the right temperature. Removal of magnesium through modern technologies can be efficiently performed to prevent environmental problems.

Platinum-group elements (Rh, Pt, Pd) and Au distribution in snow samples from the Kola Peninsula, NW Russia

NASA Astrophysics Data System (ADS)

Gregurek, Dean; Melcher, Frank; Niskavaara, Heikki; Pavlov, Vladimir A.; Reimann, Clemens; Stumpfl, Eugen F.

In April 1996 snowpack samples were collected from the surroundings of the ore roasting and dressing plant at Zapoljarnij and the nickel smelters at Nikel and Monchegorsk, Kola Peninsula, NW Russia. In the laboratory, filter residues of snowpack samples (fraction>0.45 μm) from 15 localities (close to the nickel processing centres) were chemically for precious metals (Rh, Pt, Pd, Au) and Te by graphite furnace atomic absorption spectrometry (GFAAS) analysis, and for Cu and Ni by ICP-MS. Values up to 2770 ng/l Pd, 650 ng/l Pt and 186 ng/l Au were found in the filter residues. Additionally, platinum-group elements (PGE) and Au contents in ore samples from Noril'sk , as well as in technogenic products ("Cu-Ni-feinstein" and copper concentrate) processed at the Monchegorsk smelter complex, were analysed using flameless atomic absorption spectroscopy (FAAS) for comparison with results obtained from snow. Rh, Pt, Pd and Au distribution data show the presence of two ore components (Noril'sk and Pechenga). Concentrations of these metals decrease with distance from the industrial sources and with the prevailing wind direction (generally north-south). Microscopic investigations and electron microprobe analysis of polished sections of snow filter residues (>0.45 μm) also reveal differences between particles from the two sources. To avoid confusion the term "Noril'sk" is used throughout the paper to denote material and/or data from the Noril'sk area and its sub-district, Noril'sk while Pechenga relates to the local ore.

Design Considerations for Lightweight Space Radiators Based on Fabrication and Test Experience with a Carbon-Carbon Composite Prototype Heat Pipe

NASA Technical Reports Server (NTRS)

Juhasz, Albert J.

1998-01-01

This report discusses the design implications for spacecraft radiators made possible by the successful fabrication and Proof-of-concept testing of a graphite-fiber-carbon-matrix composite (i.e., carbon-carbon (C-C)) heat pipe. The proto-type heat pipe, or space radiator element, consists of a C-C composite shell with integrally woven fins. It has a thin-walled furnace-brazed metallic (Nb-1%Zr) liner with end caps for containment of the potassium working fluid. A short extension of this liner, at increased wall thickness beyond the C-C shell, forms the heat pipe evaporator section which is in thermal contact with the radiator fluid that needs to be cooled. From geometric and thermal transport properties of the C-C composite heat pipe tested, a specific radiator mass of 1.45 kg/m2 can be derived. This is less than one-fourth the specific mass of present day satellite radiators. The report also discusses the advantage of segmented space radiator designs utilizing heat pipe elements, or segments, in their survivability to micro-meteoroid damage. This survivability is further raised by the use of condenser sections with attached fins, which also improve the radiation heat transfer rate. Since the problem of heat radiation from a fin does not lend itself to a closed analytical solution, a derivation of the governing differential equation and boundary conditions is given in appendix A, along with solutions for rectangular and parabolic fin profile geometries obtained by use of a finite difference computer code written by the author.

Design Considerations for Lightweight Space Radiators Based on Fabrication and Test Experience With a Carbon-Carbon Composite Prototype Heat Pipe. Revised

NASA Technical Reports Server (NTRS)

Juhasz, Albert J.

2002-01-01

This report discusses the design implications for spacecraft radiators made possible by the successful fabrication and proof-of-concept testing of a graphite-fiber-carbon-matrix composite (i.e., carbon-carbon (C-C)) heat pipe. The prototype heat pipe, or space radiator element, consists of a C-C composite shell with integrally woven fins. It has a thin-walled furnace-brazed metallic (Nb-1%Zr) liner with end caps for containment of the potassium working fluid. A short extension of this liner, at increased wall thickness beyond the C-C shell, forms the heat pipe evaporator section which is in thermal contact with the radiator fluid that needs to be cooled. From geometric and thermal transport properties of the C-C composite heat pipe tested, a specific radiator mass of 1.45 kg/sq m can be derived. This is less than one-fourth the specific mass of present day satellite radiators. The report also discusses the advantage of segmented space radiator designs utilizing heat pipe elements, or segments, in their survivability to micrometeoroid damage. This survivability is further raised by the use of condenser sections with attached fins, which also improve the radiation heat transfer rate. Since the problem of heat radiation from a fin does not lend itself to a closed analytical solution, a derivation of the governing differential equation and boundary conditions is given in appendix A, along with solutions for rectangular and parabolic fin profile geometries obtained by use of a finite difference computer code written by the author.

Utilization of optimized BCR three-step sequential and dilute HCl single extraction procedures for soil-plant metal transfer predictions in contaminated lands.

PubMed

Kubová, Jana; Matús, Peter; Bujdos, Marek; Hagarová, Ingrid; Medved', Ján

2008-05-30

The prediction of soil metal phytoavailability using the chemical extractions is a conventional approach routinely used in soil testing. The adequacy of such soil tests for this purpose is commonly assessed through a comparison of extraction results with metal contents in relevant plants. In this work, the fractions of selected risk metals (Al, As, Cd, Cu, Fe, Mn, Ni, Pb, Zn) that can be taken up by various plants were obtained by optimized BCR (Community Bureau of Reference) three-step sequential extraction procedure (SEP) and by single 0.5 mol L(-1) HCl extraction. These procedures were validated using five soil and sediment reference materials (SRM 2710, SRM 2711, CRM 483, CRM 701, SRM RTH 912) and applied to significantly different acidified soils for the fractionation of studied metals. The new indicative values of Al, Cd, Cu, Fe, Mn, P, Pb and Zn fractional concentrations for these reference materials were obtained by the dilute HCl single extraction. The influence of various soil genesis, content of essential elements (Ca, Mg, K, P) and different anthropogenic sources of acidification on extraction yields of individual risk metal fractions was investigated. The concentrations of studied elements were determined by atomic spectrometry methods (flame, graphite furnace and hydride generation atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry). It can be concluded that the data of extraction yields from first BCR SEP acid extractable step and soil-plant transfer coefficients can be applied to the prediction of qualitative mobility of selected risk metals in different soil systems.

Heat Transfer Coefficient Distribution in the Furnace of a 300MWe CFB Boiler

NASA Astrophysics Data System (ADS)

Zhang, P.; Lu, J. F.; Yang, H. R.; Zhang, J. S.; Zhang, H.; Yue, G. X.

Properly understanding and calculating the distributions of heat flux and heat transfer coefficient (α) in the furnace is important in designing a circulating fluidized bed (CFB) boiler, especially with supercritical parameters. Experimental study on the heat transfer in a commercial 300MWe CFB boiler was conducted. The α from the bed to the water wall was measured by the finite element method (FEM), at five different heights. The influence of suspension density and bed temperature on α was analyzed. It was found that the pressure difference between the inlet and exit of the three cyclones, and the chamber pressure of the corresponding loop seal were not equal. The results indicated the suspension solid density was non-uniform in the cross section at a certain height. Consequently, the distributions of heat flux and α in the horizontal plane in the furnace was non-uniform. The furnace can divided into three sections according to the arrangement of the platen superheaters hanging in the upper CFB furnace. In each section, the heat flux near the center showed increasing trend.

Comparison of the tribological properties of fluorinated cokes and graphites

NASA Technical Reports Server (NTRS)

Fusaro, Robert L.

1988-01-01

The friction, wear, endurance life, and surface morphology of rubbed (burnished) fluorinated graphite and fluorinated coke materials were studied. Two different coke powders, a graphitic carbon powder, and a graphite powder were fluorinated and then tribologically investigated. In addition, one of the coke powders was reduced in size before fluorinating to evaluate the effect of a finer particle size on the tribological properties. For comparison, graphite and coke powders which were not fluorinated were also tribologically evaluated. Elemental analysis by emission spectroscopy was performed on each sample to determine the impurity content and X-ray diffraction analysis was performed to determine the crystallinity. Coke was found to have very little lubricating ability, but fluorinated coke did possess good lubricating properties. However, the fluorinated graphite and fluorinated graphitic carbon (which gave equivalent results) gave superior results to those obtained with the fluorinated cokes. No tribological benefit was found for using small versus a larger particle size of coke, at least when evaluated as a rubbed film.

Comparison of the tribological properties of fluorinated cokes and graphites

NASA Technical Reports Server (NTRS)

Fusaro, Robert L.

1987-01-01

The friction, wear, endurance life, and surface morphology of rubbed (burnished) fluorinated graphite and fluorinated coke materials were studied. Two different coke powders, a graphitic carbon powder, and a graphite powder were fluorinated and then tribologically investigated. In addition, one of the coke powders was reduced in size before fluorinating to evaluate the effect of a finer particle size on the tribological properties. For comparison, graphite and coke powders which were not fluorinated were also tribologically evaluated. Elemental analysis by emission spectroscopy was performed on each sample to determine the impurity content and X-ray diffraction analysis was performed to determine the crystallinity. Coke was found to have very little lubricating ability, but fluorinated coke did possess good lubricating properties. However, the fluorinated graphite and fluorinated graphitic carbon (which gave equivalent results) gave superior results to those obtained with the fluorinated cokes. No tribological benefit was found for using small versus a larger particle size of coke, at least when evaluated as a rubbed film.

High temperature gas-cooled reactor (HTGR) graphite pebble fuel: Review of technologies for reprocessing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mcwilliams, A. J.

2015-09-08

This report reviews literature on reprocessing high temperature gas-cooled reactor graphite fuel components. A basic review of the various fuel components used in the pebble bed type reactors is provided along with a survey of synthesis methods for the fabrication of the fuel components. Several disposal options are considered for the graphite pebble fuel elements including the storage of intact pebbles, volume reduction by separating the graphite from fuel kernels, and complete processing of the pebbles for waste storage. Existing methods for graphite removal are presented and generally consist of mechanical separation techniques such as crushing and grinding chemical techniquesmore » through the use of acid digestion and oxidation. Potential methods for reprocessing the graphite pebbles include improvements to existing methods and novel technologies that have not previously been investigated for nuclear graphite waste applications. The best overall method will be dependent on the desired final waste form and needs to factor in the technical efficiency, political concerns, cost, and implementation.« less

Investigations on Mechanical Behaviour of Micro Graphite Particulates Reinforced Al-7Si Alloy Composites

NASA Astrophysics Data System (ADS)

Nagaraj, N.; Mahendra, K. V.; Nagaral, Madeva

2018-02-01

Micro particulates reinforced metal matrix composites are finding wide range of applications in automotive and sports equipment manufacturing industries. In the present study, an attempt has been made to develop Al-7Si-micro graphite particulates reinforced composites by using liquid melt method. 3 and 6 wt. % of micro graphite particulates were added to the Al-7Si base matrix. Microstructural characterization was done by using scanning electron microscope and energy dispersive spectroscope. Mechanical behaviour of Al-7Si-3 and 6 wt. % composites were evaluated as per ASTM standards. Scanning electron micrographs revealed the uniform distribution of micro graphite particulates in the Al-7Si alloy matrix. EDS analysis confirmed the presence of B and C elements in graphite reinforced composites. Further, it was noted that ultimate tensile and yield strength of Al-7Si alloy increased with the addition of 3 and 6wt. % of graphite particulates. Hardness of graphite reinforced composites was lesser than the base matrix.

New method for the direct determination of dissolved Fe(III) concentration in acid mine waters

USGS Publications Warehouse

To, T.B.; Nordstrom, D. Kirk; Cunningham, K.M.; Ball, J.W.; McCleskey, R. Blaine

1999-01-01

A new method for direct determination of dissolved Fe(III) in acid mine water has been developed. In most present methods, Fe(III) is determined by computing the difference between total dissolved Fe and dissolved Fe(II). For acid mine waters, frequently Fe(II) >> Fe(III); thus, accuracy and precision are considerably improved by determining Fe(III) concentration directly. The new method utilizes two selective ligands to stabilize Fe(III) and Fe(II), thereby preventing changes in Fe reduction-oxidation distribution. Complexed Fe(II) is cleanly removed using a silica-based, reversed-phase adsorbent, yielding excellent isolation of the Fe(III) complex. Iron(III) concentration is measured colorimetrically or by graphite furnace atomic absorption spectrometry (GFAAS). The method requires inexpensive commercial reagents and simple procedures that can be used in the field. Calcium(II), Ni(II), Pb(II), AI(III), Zn(II), and Cd(II) cause insignificant colorimetric interferences for most acid mine waters. Waters containing >20 mg of Cu/L could cause a colorimetric interference and should be measured by GFAAS. Cobalt(II) and Cr(III) interfere if their molar ratios to Fe(III) exceed 24 and 5, respectively. Iron(II) interferes when its concentration exceeds the capacity of the complexing ligand (14 mg/L). Because of the GFAAS elemental specificity, only Fe(II) is a potential interferent in the GFAAS technique. The method detection limit is 2 ??g/L (40 nM) using GFAAS and 20 ??g/L (0.4 ??M) by colorimetry.A new method for direct determination of dissolved Fe(III) in acid mine water has been developed. In most present methods, Fe(III) is determined by computing the difference between total dissolved Fe and dissolved Fe(II). For acid mine waters, frequently Fe(II)???Fe(III); thus, accuracy and precision are considerably improved by determining Fe(III) concentration directly. The new method utilizes two selective ligands to stabilize Fe(III) and Fe(II), thereby preventing changes in Fe reduction-oxidation distribution. Complexed Fe(II) is cleanly removed using a silica-based, reversed-phase adsorbent, yielding excellent isolation of the Fe(III) complex. Iron(III) concentration is measured colorimetrically or by graphite furnace atomic absorption spectrometry (GFAAS). The method requires inexpensive commercial reagents and simple procedures that can be used in the field. Calcium(II), Ni(II), Pb(II), Al(III), Zn(II), and Cd(II) cause insignificant colorimetric interferences for most acid mine waters. Waters containing >20 mg of Cu/L could cause a colorimetric interference and should be measured by GFAAS. Cobalt(II) and Cr(III) interfere if their molar ratios to Fe(III) exceed 24 and 5, respectively. Iron(II) interferes when its concentration exceeds the capacity of the complexing ligand (14 mg/L). Because of the GFAAS elemental specificity, only Fe(II) is a potential interferent in the GFAAS technique. The method detection limit is 2/??g/L (40 nM) using GFAAS and 20 ??g/L (0.4 ??M) by colorimetry.

Ion irradiation induced defect evolution in Ni and Ni-based FCC equiatomic binary alloys

DOE PAGES

Jin, Ke; Zhang, Yanwen; Bei, Hongbin

2015-09-09

In order to explore the chemical effects on radiation response of alloys with multi-principal elements, defect evolution under Au ion irradiation was investigated in the elemental Ni, equiatomic NiCo and NiFe alloys. Single crystals were successfully grown in an optical floating zone furnace and their (100) surfaces were irradiated with 3 MeV Au ions at fluences ranging from 1 × 10 13 to 5 × 10 15 ions cm –2 at room temperature. The irradiation-induced defect evolution was analyzed by using ion channeling technique. Experiment shows that NiFe is more irradiation-resistant than NiCo and pure Ni at low fluences. Withmore » continuously increasing the ion fluences, damage level is eventually saturated for all materials but at different dose levels. The saturation level in pure Ni appears at relatively lower irradiation fluence than the alloys, suggesting that damage accumulation slows down in the alloys. Here, under high-fluence irradiations, pure Ni has wider damage ranges than the alloys, indicating that defects in pure Ni have high mobility.« less

Interstellar grains within interstellar grains

NASA Technical Reports Server (NTRS)

Bernatowicz, Thomas J.; Amari, Sachiko; Zinner, Ernst K.; Lewis, Roy S.

1991-01-01

Five interstellar graphite spherules extracted from the Murchison carbonaceous meteorite are studied. The isotopic and elemental compositions of individual particles are investigated with the help of an ion microprobe, and this analysis is augmented with structural studies of ultrathin sections of the grain interiors by transmission electron microscopy. As a result, the following procedure for the formation of the interstellar graphite spherule bearing TiC crystals is inferred: (1) high-temperature nucleation and rapid growth of the graphitic carbon spherule in the atmosphere of a carbon-rich star, (2) nucleation and growth of TiC crystals during continued growth of the graphitic spherule and the accretion of TiC onto the spherule, (3) quenching of the graphite growth process by depletion of C or by isolation of the spherule before other grain types could condense.

Structural stiffness, strength and dynamic characteristics of large tetrahedral space truss structures

NASA Technical Reports Server (NTRS)

Mikulas, M. M., Jr.; Bush, H. G.; Card, M. F.

1977-01-01

Physical characteristics of large skeletal frameworks for space applications are investigated by analyzing one concept: the tetrahedral truss, which is idealized as a sandwich plate with isotropic faces. Appropriate analytical relations are presented in terms of the truss column element properties which for calculations were taken as slender graphite/epoxy tubes. Column loads, resulting from gravity gradient control and orbital transfer, are found to be small for the class structure investigated. Fundamental frequencies of large truss structures are shown to be an order of magnitude lower than large earth based structures. Permissible loads are shown to result in small lateral deflections of the truss due to low-strain at Euler buckling of the slender graphite/epoxy truss column elements. Lateral thermal deflections are found to be a fraction of the truss depth using graphite/epoxy columns.

Microwave limb sounder, graphite epoxy support structure

NASA Technical Reports Server (NTRS)

Pynchon, G.

1980-01-01

The manufacturing and processing procedures which were used to fabricate a precision graphite/epoxy support structure for a spherical microwave reflecting surface are described. The structure was made fromm GY-70/930 ultra high modulus graphite prepreg, laminated to achieve an isotropic in plane thermal expansion of less than + or - 0.1 PPM/F. The structure was hand assembled to match the interface of the reflective surface, which was an array of 18 flexure supported, aluminum, spherically contoured tiles. Structural adhesives were used in the final assembly to bond the elements into their final configuration. A eutectic metal coating was applied to the composite surface to reduce dimensional instabilities arising from changes in the composite epoxy moisture content due to environmental effects. Basic materials properties data are reported and the results of a finite element structural analysis are referenced.

B and N isolate-doped graphitic carbon nanosheets from nitrogen-containing ion-exchanged resins for enhanced oxygen reduction

NASA Astrophysics Data System (ADS)

Wang, Lei; Yu, Peng; Zhao, Lu; Tian, Chungui; Zhao, Dongdong; Zhou, Wei; Yin, Jie; Wang, Ruihong; Fu, Honggang

2014-06-01

B,N-codoped carbon nanostructures (BNCS) can serve as alternative low-cost metal-free electrocatalysts for oxygen reduction reactions (ORR). However, the compensation effect between the p- (B atoms) and n-type (N atoms) dopants would make the covalent boron-nitride (BN) easily formed during the synthesis of BNCS, leading to a unsatisfactory ORR activity. Therefore, it has been challenging to develop facile and rapid synthetic strategies for highly active BNCS without forming the direct covalent BN. Here, a facile method is developed to prepare B and N isolate-doped graphitic nanosheets (BNGS) by using iron species for saving N element and simultaneous doping the B element from nitrogen-containing ion-exchanged resins (NR). The resulting BNGS exhibits much more onset potential (Eonset) compared with the B-doped graphitic carbon nanosheets (BGS), N-doped graphitic carbon nanosheets (NGS), as well as B,N-codoped disorder carbon (BNC). Moreover, the BNGS shows well methanol tolerance propery and excellent stability (a minimal loss of activity after 5,000 potential cycles) compared to that of commercial Pt/C catalyst. The goog performance for BNGS towards ORR is attributed to the synergistic effect between B and N, and the well electrons transport property of graphitic carbon in BNGS.

Methods for detecting the mobility of trace elements during medium-temperature pyrolysis

USGS Publications Warehouse

Shiley, R.H.; Konopka, K.L.; Cahill, R.A.; Hinckley, C.C.; Smith, Gerard V.; Twardowska, H.; Saporoschenko, Mykola

1983-01-01

The mobility (volatility) of trace elements in coal during pyrolysis has been studied for distances of up to 40 cm between the coal and the trace element collector, which was graphite or a baffled solvent trap. Nineteen elements not previously recorded as mobile were detected. ?? 1983.

A New Method to Measure Crack Extension in Nuclear Graphite Based on Digital Image Correlation

DOE PAGES

Lai, Shigang; Shi, Li; Fok, Alex; ...

2017-01-01

Graphite components, used as moderators, reflectors, and core-support structures in a High-Temperature Gas-Cooled Reactor, play an important role in the safety of the reactor. Specifically, they provide channels for the fuel elements, control rods, and coolant flow. Fracture is the main failure mode for graphite, and breaching of the above channels by crack extension will seriously threaten the safety of a reactor. In this paper, a new method based on digital image correlation (DIC) is introduced for measuring crack extension in brittle materials. Cross-correlation of the displacements measured by DIC with a step function was employed to identify the advancingmore » crack tip in a graphite beam specimen under three-point bending. The load-crack extension curve, which is required for analyzing the R-curve and tension softening behaviors, was obtained for this material. Furthermore, a sensitivity analysis of the threshold value employed for the cross-correlation parameter in the crack identification process was conducted. Finally, the results were verified using the finite element method.« less

A New Method to Measure Crack Extension in Nuclear Graphite Based on Digital Image Correlation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lai, Shigang; Shi, Li; Fok, Alex

Graphite components, used as moderators, reflectors, and core-support structures in a High-Temperature Gas-Cooled Reactor, play an important role in the safety of the reactor. Specifically, they provide channels for the fuel elements, control rods, and coolant flow. Fracture is the main failure mode for graphite, and breaching of the above channels by crack extension will seriously threaten the safety of a reactor. In this paper, a new method based on digital image correlation (DIC) is introduced for measuring crack extension in brittle materials. Cross-correlation of the displacements measured by DIC with a step function was employed to identify the advancingmore » crack tip in a graphite beam specimen under three-point bending. The load-crack extension curve, which is required for analyzing the R-curve and tension softening behaviors, was obtained for this material. Furthermore, a sensitivity analysis of the threshold value employed for the cross-correlation parameter in the crack identification process was conducted. Finally, the results were verified using the finite element method.« less

High temperature spectral emissivity measurement using integral blackbody method

NASA Astrophysics Data System (ADS)

Pan, Yijie; Dong, Wei; Lin, Hong; Yuan, Zundong; Bloembergen, Pieter

2016-10-01

Spectral emissivity is a critical material's thermos-physical property for heat design and radiation thermometry. A prototype instrument based upon an integral blackbody method was developed to measure material's spectral emissivity above 1000 °. The system was implemented with an optimized commercial variable-high-temperature blackbody, a high speed linear actuator, a linear pyrometer, and an in-house designed synchronization circuit. A sample was placed in a crucible at the bottom of the blackbody furnace, by which the sample and the tube formed a simulated blackbody which had an effective total emissivity greater than 0.985. During the measurement, the sample was pushed to the end opening of the tube by a graphite rod which was actuated through a pneumatic cylinder. A linear pyrometer was used to monitor the brightness temperature of the sample surface through the measurement. The corresponding opto-converted voltage signal was fed and recorded by a digital multi-meter. A physical model was proposed to numerically evaluate the temperature drop along the process. Tube was discretized as several isothermal cylindrical rings, and the temperature profile of the tube was measurement. View factors between sample and rings were calculated and updated along the whole pushing process. The actual surface temperature of the sample at the end opening was obtained. Taking advantages of the above measured voltage profile and the calculated true temperature, spectral emissivity under this temperature point was calculated.

Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

2015-08-01

A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

Dynamic responses of graphite/epoxy laminated beam to impact of elastic spheres

NASA Technical Reports Server (NTRS)

Sun, C. T.; Wang, T.

1982-01-01

Wave propagation in 90/45/90/-45/902s and 0/45/0/-45/02s laminates of a graphite/epoxy composite due to impact of a steel ball was investigated experimentally and also by using a high order beam finite element. Dynamic strain responses at several locations were obtained using strain gages. The finite element program which incorporated statically determined contact laws was employed to calculate the contact force history as well as the target beam dynamic deformation. The comparison of the finite element solutions with the experimental data indicated that the static contact laws for loading and unloading (developed under this grant) are adequate for the dynamic impact analysis. It was found that for the 0/45/0/-45/02s laminate which has a much larger longitudinal bending rigidity, the use of beam finite elements is not suitable and plate finite element should be used instead.

AOD furnace splash soft-sensor in the smelting process based on improved BP neural network

NASA Astrophysics Data System (ADS)

Ma, Haitao; Wang, Shanshan; Wu, Libin; Yu, Ying

2017-11-01

In view of argon oxygen refining low carbon ferrochrome production process, in the splash of smelting process as the research object, based on splash mechanism analysis in the smelting process , using multi-sensor information fusion and BP neural network modeling techniques is proposed in this paper, using the vibration signal, the audio signal and the flame image signal in the furnace as the characteristic signal of splash, the vibration signal, the audio signal and the flame image signal in the furnace integration and modeling, and reconstruct splash signal, realize the splash soft measurement in the smelting process, the simulation results show that the method can accurately forecast splash type in the smelting process, provide a new method of measurement for forecast splash in the smelting process, provide more accurate information to control splash.

Influence of crucible support and radial heating on the interface shape during vertical Bridgman GaAs growth

NASA Astrophysics Data System (ADS)

Koai, K.; Sonnenberg, K.; Wenzl, H.

1994-03-01

Crucible assembly in a vertical Bridgman furnace is investigated by a numerical finite element model with the aim to obtain convex interfaces during the growth of GaAs crystals. During the growth stage of the conic section, a new funnel shaped crucible support has been found more effective than the concentric cylinders design similar to that patented by AT & T in promoting interface convexity. For the growth stages of the constant diameter section, the furnace profile can be effectively modulated by localized radial heating at the gradient zone. With these two features being introduced into a new furnace design, it is shown numerically that enhancement of interface convexity can be achieved using the presently available crucible materials.

Development of a Continuum Damage Mechanics Material Model of a Graphite-Kevlar(Registered Trademark) Hybrid Fabric for Simulating the Impact Response of Energy Absorbing Kevlar(Registered Trademark) Hybrid Fabric for Simulating the Impact Response of Energy Absorbing

NASA Technical Reports Server (NTRS)

Jackson, Karen E.; Fasanella, Edwin L.; Littell, Justin D.

2017-01-01

This paper describes the development of input properties for a continuum damage mechanics based material model, Mat 58, within LS-DYNA(Registered Trademark) to simulate the response of a graphite-Kevlar(Registered Trademark) hybrid plain weave fabric. A limited set of material characterization tests were performed on the hybrid graphite-Kevlar(Registered Trademark) fabric. Simple finite element models were executed in LS-DYNA(Registered Trademark) to simulate the material characterization tests and to verify the Mat 58 material model. Once verified, the Mat 58 model was used in finite element models of two composite energy absorbers: a conical-shaped design, designated the "conusoid," fabricated of four layers of hybrid graphite-Kevlar(Registered Trademark) fabric; and, a sinusoidal-shaped foam sandwich design, designated the "sinusoid," fabricated of the same hybrid fabric face sheets with a foam core. Dynamic crush tests were performed on components of the two energy absorbers, which were designed to limit average vertical accelerations to 25- to 40-g, to minimize peak crush loads, and to generate relatively long crush stroke values under dynamic loading conditions. Finite element models of the two energy absorbers utilized the Mat 58 model that had been verified through material characterization testing. Excellent predictions of the dynamic crushing response were obtained.

Application of graphite as a geothermometer in hydrothermally altered metamorphic rocks of the Merelani-Lelatema area, Mozambique Belt, northeastern Tanzania

NASA Astrophysics Data System (ADS)

Malisa, Elias Pausen

1998-02-01

Upper Precambrian pelitic and psammitic gneisses in the Mozambique Belt are usually graphite rich. The determination of crystallisation temperatures around and in the hydrothermally altered rocks of the Merelani-Lelatema mining areas, northeastern Tanzania, were made by studying the lattice parameter C of graphite. In this way, the migration of the chromophore elements giving colour to the gemstones, e.g. tanzanite, green garnet and green tourmaline in the area, can be studied. Within the hydrothermally altered zone graphite gives temperatures that range from 523°C to 880°C. These temperatures are much higher than the 390-440°C obtained through fluid inclusion studies of tanzanite, which indicates that the graphite was not hydrothermally introduced. Furthermore the hydrothermal solutions are post-metamorphic.

Extraction and speciation of arsenic in lacustrine sediments

USGS Publications Warehouse

Ficklin, W.H.

1990-01-01

Arsenic was partially extracted with 4.OM hydrochloric acid, from samples collected at 25-cm intervals in a 350-cm column of sediment at Milltown Reservoir, Montana and from a 60-cm core of sediment collected at the Cheyenne River Embayment of Lake Oahe, South Dakota. The sediment in both reservoirs is highly contaminated with arsenic. The extracted arsenic was separated into As(III) and As(V) on acetate form Dowex 1-X8 ion-exchange resin with 0.12M HCl eluent. Residual arsenic was sequentially extracted with KClO3 and HCl. Arsenic was determined by graphite-furnace atomic-absorption spectrometry. The analytical results define oxidized and reduced zones in the sediment columns. ?? 1990.

Final Summary of Research Report to the National Aeronautics and Space Administration Cosmochemistry Program

NASA Technical Reports Server (NTRS)

O'D. Alexander, Conel

2003-01-01

The discovery of presolar grains in meteorites is one of the most exciting recent developments in meteoritics. Six types of presolar grain have been discovered: diamond, Sic, graphite, Si3N4, Al2O3 and MgAl2O4. These grains have been identified as presolar because their isotopic compositions are very different from those of Solar System materials. Comparison of their isotopic compositions with astronomical observations and theoretical models indicates most of the grains formed in the envelopes of highly evolved stars. They are, therefore, a new source of information with which to test astrophysical models of the evolution of these stars. In fact, because several elements can often be measured in the same grain, including elements that are not measurable spectroscopically in stars, the grain data provide some very stringent constraints for these models. Our primary goal is to create large, unbiased, multi-isotope databases of single presolar Sic, Si,N,, oxide and graphite grains in meteorites, as well as any new presolar grain types that are identified in the future. These will be used to: (i) test stellar and nucleosynthetic models, (ii) constrain the galactic chemical evolution (GCE) paths of the isotopes of Si, Ti, O and Mg, (iii) establish how many stellar sources contributed to the Solar System, (iv) constrain relative dust production rates of various stellar types and (v) assess how representative of galactic dust production the record in meteorites is. The primary tool for this project is a highly automated grain analysis system on the Carnegie 6f ion probe.

Final Summary of Research Report to the National Aeronautics and Space Administration Cosmochemistry Program

NASA Technical Reports Server (NTRS)

O'D.Alexander, Conel

2004-01-01

The discovery of presolar grains in meteorites is one of the most exciting recent developments in meteoritics. Six types of presolar grain have been discovered: diamond, Sic, graphite, Si3N4, Al2O3 and MgAl2O4. These grains have been identified as presolar because their isotopic compositions are very different from those of Solar System materials. Comparison of their isotopic compositions with astronomical observations and theoretical models indicates most of the grains formed in the envelopes of highly evolved stars. They are, therefore, a new source of information with which to test astrophysical models of the evolution of these stars. In fact, because several elements can often be measured in the same grain, including elements that are not measurable spectroscopically in stars, the grain data provide some very stringent constraints for these models. Our primary goal is to create large, unbiased, multi-isotope databases of single presolar Sic, Si,N,, oxide and graphite grains in meteorites, as well as any new presolar grain types that are identified in the future. These will be used to: (i) test stellar and nucleosynthetic models, (ii) constrain the galactic chemical evolution (GCE) paths of the isotopes of Si, Ti, 0 and Mg, (iii) establish how many stellar sources contributed to the Solar System, (iv) constrain relative dust production rates of various stellar types and (v) assess how representative of galactic dust production the record in meteorites is. The primary tool for this project is a highly automated grain analysis system we have developed for the Carnegie 6f ion probe.

FUEL ASSAY REACTOR

DOEpatents

Spinrad, B.I.; Sandmeier, H.A.; Martens, F.H.

1962-12-25

A reactor having maximum sensitivity to perturbations is described comprising a core consisting of a horizontally disposed, rectangular, annular fuel zone containing enriched uranium dioxide dispersed in graphite, the concentration of uranium dioxide increasing from the outside to the inside of the fuel zone, an internal reflector of graphite containing an axial test opening disposed within the fuel zone, an external graphite reflector, means for changing the neutron spectrum in the test opening, and means for measuring perturbations in the neutron flux caused by the introduction of different fuel elements into the test opening. (AEC)

A Novel Ultrafast Rechargeable Multi-Ions Battery.

PubMed

Wang, Shuai; Jiao, Shuqiang; Tian, Donghua; Chen, Hao-Sen; Jiao, Handong; Tu, Jiguo; Liu, Yingjun; Fang, Dai-Ning

2017-04-01

An ultrafast rechargeable multi-ions battery is presented, in which multi-ions can electrochemically intercalate into graphite layers, exhibiting a high reversible discharge capacity of ≈100 mAh g -1 and a Coulombic efficiency of ≈99% over hundreds of cycles at a high current density. The results may open up a new paradigm for multi-ions-based electrochemical battery technologies and applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Composites of aluminum alloy and magnesium alloy with graphite showing low thermal expansion and high specific thermal conductivity

NASA Astrophysics Data System (ADS)

Oddone, Valerio; Boerner, Benji; Reich, Stephanie

2017-12-01

High thermal conductivity, low thermal expansion and low density are three important features in novel materials for high performance electronics, mobile applications and aerospace. Spark plasma sintering was used to produce light metal-graphite composites with an excellent combination of these three properties. By adding up to 50 vol.% of macroscopic graphite flakes, the thermal expansion coefficient of magnesium and aluminum alloys was tuned down to zero or negative values, while the specific thermal conductivity was over four times higher than in copper. No degradation of the samples was observed after thermal stress tests and thermal cycling. Tensile strength and hardness measurements proved sufficient mechanical stability for most thermal management applications. For the production of the alloys, both prealloyed powders and elemental mixtures were used; the addition of trace elements to cope with the oxidation of the powders was studied.

Composites of aluminum alloy and magnesium alloy with graphite showing low thermal expansion and high specific thermal conductivity

PubMed Central

Oddone, Valerio; Boerner, Benji; Reich, Stephanie

2017-01-01

Abstract High thermal conductivity, low thermal expansion and low density are three important features in novel materials for high performance electronics, mobile applications and aerospace. Spark plasma sintering was used to produce light metal–graphite composites with an excellent combination of these three properties. By adding up to 50 vol.% of macroscopic graphite flakes, the thermal expansion coefficient of magnesium and aluminum alloys was tuned down to zero or negative values, while the specific thermal conductivity was over four times higher than in copper. No degradation of the samples was observed after thermal stress tests and thermal cycling. Tensile strength and hardness measurements proved sufficient mechanical stability for most thermal management applications. For the production of the alloys, both prealloyed powders and elemental mixtures were used; the addition of trace elements to cope with the oxidation of the powders was studied. PMID:28458742

Composites of aluminum alloy and magnesium alloy with graphite showing low thermal expansion and high specific thermal conductivity.

PubMed

Oddone, Valerio; Boerner, Benji; Reich, Stephanie

2017-01-01

High thermal conductivity, low thermal expansion and low density are three important features in novel materials for high performance electronics, mobile applications and aerospace. Spark plasma sintering was used to produce light metal-graphite composites with an excellent combination of these three properties. By adding up to 50 vol.% of macroscopic graphite flakes, the thermal expansion coefficient of magnesium and aluminum alloys was tuned down to zero or negative values, while the specific thermal conductivity was over four times higher than in copper. No degradation of the samples was observed after thermal stress tests and thermal cycling. Tensile strength and hardness measurements proved sufficient mechanical stability for most thermal management applications. For the production of the alloys, both prealloyed powders and elemental mixtures were used; the addition of trace elements to cope with the oxidation of the powders was studied.

Design fabrication and test of graphite/polyimide composite joints and attachments for advanced aerospace vehicles

NASA Technical Reports Server (NTRS)

1979-01-01

Graphite/polyimide (Gr/PI) bolted and bonded joints were investigated. Possible failure modes and the design loads for the four generic joint types are discussed. Preliminary sizing of a type 1 joint, bonded and bolted configuration is described, including assumptions regarding material properties and sizing methodology. A general purpose finite element computer code is described that was formulated to analyze single and double lap joints, with and without tapered adherends, and with user-controlled variable element size arrangements. An initial order of Celion 6000/PMR-15 prepreg was received and characterized.

Stress analysis and buckling of J-stiffened graphite-epoxy panel

NASA Technical Reports Server (NTRS)

Davis, R. C.

1980-01-01

A graphite epoxy shear panel with bonded on J stiffeners was investigated. The panel, loaded to buckling in a picture frame shear test is described. Two finite element models, each of which included the doubler material bonded to the panel skin under the stiffeners and at the panel edges, were used to make a stress analysis of the panel. The shear load distributions in the panel from two commonly used boundary conditions, applied shear load and applied displacement, were compared with the results from one of the finite element models that included the picture frame test fixture.

Balanced improvement of high performance concrete material properties with modified graphite nanomaterials

NASA Astrophysics Data System (ADS)

Peyvandi, Amirpasha

Graphite nanomaterials offer distinct features for effective reinforcement of cementitious matrices in the pre-crack and post-crack ranges of behavior. Thoroughly dispersed and well-bonded nanomaterials provide for effective control of the size and propagation of defects (microcracks) in matrix, and also act as closely spaced barriers against diffusion of moisture and aggressive solutions into concrete. Modified graphite nanomaterials can play multi-faceted roles towards enhancing the mechanical, physical and functional attributes of concrete materials. Graphite nanoplatelets (GP) and carbon nanofibers (CNF) were chosen for use in cementitious materials. Experimental results highlighted the balanced gains in diverse engineering properties of high-performance concrete realized by introduction of graphite nanomaterials. Nuclear Magnetic Resonance (NMR) spectroscopy was used in order to gain further insight into the effects of nanomaterials on the hydration process and structure of cement hydrates. NMR exploits the magnetic properties of certain atomic nuclei, and the sensitivity of these properties to local environments to generate data which enables determination of the internal structure, reaction state, and chemical environment of molecules and bulk materials. 27 Al and 29Si NMR spectroscopy techniques were employed in order to evaluate the effects of graphite nanoplatelets on the structure of cement hydrates, and their resistance to alkali-silica reaction (ASR), chloride ion diffusion, and sulfate attack. Results of 29Si NMR spectroscopy indicated that the percent condensation of C-S-H in cementitious paste was lowered in the presence of nanoplatelets at the same age. The extent of chloride diffusion was assessed indirectly by detecting Friedel's salt as a reaction product of chloride ions with aluminum-bearing cement hydrates. Graphite nanoplatelets were found to significantly reduce the concentration of Friedel's salt at different depths after various periods of exposure to chloride solutions, pointing at the benefits of nanoplatelets towards enhancement of concrete resistance to chloride ion diffusion. It was also found that the intensity of Thaumasite, a key species marking sulfate attack on cement hydrates, was lowered with the addition of graphite nanoplatelets in concrete exposed to sulfate solutions. Experimental evaluations were conducted on scaled-up production of concrete nanocomposite in precast concrete plants. Full-scale reinforced concrete pipes and beams were produced using concrete nanocomposites. Durability and structural tests indicated that the use of graphite nanoplatelets, alone or in combination with synthetic (PVA) fibers, produced significant gains in the durability characteristics, and also benefited the structural performance of precast reinforced concrete products. The material and scaled-up structural investigations conducted in the project concluded that lower-cost graphite nanomaterials (e.g., graphite nanoplatelets) offer significant potentials as multi-functional additives capable of enhancing the barrier, durability and mechanical performance of concrete materials. The benefits of graphite nanomaterials tend to be more pronounced in higher-performance concrete materials.

A Rapid Microwave-Assisted Thermolysis Route to Highly Crystalline Carbon Nitrides for Efficient Hydrogen Generation.

PubMed

Guo, Yufei; Li, Jing; Yuan, Yupeng; Li, Lu; Zhang, Mingyi; Zhou, Chenyan; Lin, Zhiqun

2016-11-14

Highly crystalline graphitic carbon nitride (g-C 3 N 4 ) with decreased structural imperfections benefits from the suppression of electron-hole recombination, which enhances its hydrogen generation activity. However, producing such g-C 3 N 4 materials by conventional heating in an electric furnace has proven challenging. Herein, we report on the synthesis of high-quality g-C 3 N 4 with reduced structural defects by judiciously combining the implementation of melamine-cyanuric acid (MCA) supramolecular aggregates and microwave-assisted thermolysis. The g-C 3 N 4 material produced after optimizing the microwave reaction time can effectively generate H 2 under visible-light irradiation. The highest H 2 evolution rate achieved was 40.5 μmol h -1 , which is two times higher than that of a g-C 3 N 4 sample prepared by thermal polycondensation of the same supramolecular aggregates in an electric furnace. The microwave-assisted thermolysis strategy is simple, rapid, and robust, thereby providing a promising route for the synthesis of high-efficiency g-C 3 N 4 photocatalysts. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kelli Kazuberns; Sushil Gupta; Mihaela Grigore

Blast furnace efficiency may be improved by optimizing coke reactivity. Some but not all forms of mineral matter in the coke modify its reactivity, but changes in mineral matter that occur within coke while in the blast furnace have not been fully quantified. To determine changes in mineral matter forms in the blast furnace, coke samples from a dissection study in the LKAB experimental blast furnace (EBF) were characterized using SEM/EDS analysis, EPMA (microprobe), and low-temperature ashing/quantitative XRD analysis. Variations in alkali concentration, particularly potassium, dominated the compositional changes. At high concentrations of potassium, the mineral matter was largely potassium-bearingmore » but even more potassium was diffused throughout the coke and not associated with mineral matter. There was little difference in potassium concentration between the core and surface of the coke pieces, suggesting that potassium diffused rapidly through the whole coke. Iron, calcium, silicon, and aluminum concentrations were relatively constant in comparison, although the mineralogy of all elements changed significantly with changing temperature. 23 refs., 20 figs., 9 tabs.« less

Processing, Microstructure, and Mechanical Properties of Interpenetrating Biomorphic Graphite/Copper Composites

NASA Astrophysics Data System (ADS)

Childers, Amanda Esther Sall

Composite properties can surpass those of the individual phases, allowing for the development of advanced, high-performance materials. Bio-inspired and naturally-derived materials have garnered attention as composite constituents due to their inherently efficient and complex structures. Wood-derived ceramics, produced by converting a wood precursor into a ceramic scaffold, can exhibit a wide range of microstructures depending on the wood species, including porosity, pore size and distribution, and connectivity. The focus of this work was to investigate the processing, microstructure, and properties of graphite/copper composites produced using wood-derived graphite scaffolds. Graphite/copper composites combine low specific gravity, high thermal conductivity, and tailorable thermal expansion properties, and due to the non-wetting behavior of copper to graphite, offer a unique system in which mechanically bonded interfaces in composites can be studied. Graphite scaffolds were produced from red oak, beech, and pine precursors using a catalytic pyrolyzation method, resulting in varying types of pore networks. Two infiltration methods were investigated to overcome challenges associated with non-wetting systems: copper electrodeposition and pressure-assisted melt infiltration. The phase distributions, constituent properties, interfacial characteristics, mechanical behavior, and load partitioning of these biomorphic graphite/copper composites were investigated, and were correlated to the wood species. The multi-domain feature sizes in the graphite scaffolds resulted in composites with copper relegated not only to the large, connected channels produced from the transport features in the wood, but also within the smaller, lower aspect ratio fibrous regions of the scaffold. Both features contributed to the mechanical behavior of the composites to varying degrees depending on the wood species. A multi-component predictive model also was developed and used to guide the additive-assisted electroplating of the graphitized scaffold, and helped illuminate the roles of plating additives in macro-sized channels. The model can be adapted for many material systems, sample geometries, and plating conditions to investigate the use of metal electrodeposition as a means of scaffold infiltration. Additionally, X-ray diffraction tomography was used to resolve position-dependent strain in a composite. The results of this nascent capability were discussed with respect to a two-component system under increasing uniaxial load, and compared to the results of conventional volume-averaged measurements.

Carbon Nanotubes Growth on Graphite Fibers

NASA Technical Reports Server (NTRS)

Zhu, Shen; Su, Ching-Hua; Lehoczky, S. L.; Muntele, I.; Ila, D.; Curreri, Peter A. (Technical Monitor)

2002-01-01

Carbon nanotubes (CNT) were synthesized on graphite fibers by thermal Chemical Vapor Deposition (CVD). On the fiber surface, iron nanoparticles are coated and act as catalysts for CNT growth. The growth temperature ranges from 550 to 1000 C at an ambient pressure. Methane and hydrogen gases with methane contents of 10% to 100% are used for the CNT synthesis. At high growth temperatures (greater than 800 C), the rapid inter-diffusion of the transition metal iron on the graphite surface results in a rough fiber surface with no CNT grown on the surface. When the growth temperature is relatively low (650 - 800 C), CNT are fabricated on the graphite surface with catalytic particles on the nanotube top ends. Using micro Raman spectroscopy in the breath mode region, single-walled or multi-walled CNT can be determined, depending on methane concentrations.

Kinetics of Chronic Oxidation of NBG-17 Nuclear Graphite by Water Vapor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Contescu, Cristian I; Burchell, Timothy D; Mee, Robert

2015-05-01

This report presents the results of kinetic measurements during accelerated oxidation tests of NBG-17 nuclear graphite by low concentration of water vapor and hydrogen in ultra-high purity helium. The objective is to determine the parameters in the Langmuir-Hinshelwood (L-H) equation describing the oxidation kinetics of nuclear graphite in the helium coolant of high temperature gas-cooled reactors (HTGR). Although the helium coolant chemistry is strictly controlled during normal operating conditions, trace amounts of moisture (predictably < 0.2 ppm) cannot be avoided. Prolonged exposure of graphite components to water vapor at high temperature will cause very slow (chronic) oxidation over the lifetimemore » of graphite components. This behavior must be understood and predicted for the design and safe operation of gas-cooled nuclear reactors. The results reported here show that, in general, oxidation by water of graphite NBG-17 obeys the L-H mechanism, previously documented for other graphite grades. However, the characteristic kinetic parameters that best describe oxidation rates measured for graphite NBG-17 are different than those reported previously for grades H-451 (General Atomics, 1978) and PCEA (ORNL, 2013). In some specific conditions, certain deviations from the generally accepted L-H model were observed for graphite NBG-17. This graphite is manufactured in Germany by SGL Carbon Group and is a possible candidate for the fuel elements and reflector blocks of HTGR.« less

Electrical Connector for Graphite Heating Elements

NASA Technical Reports Server (NTRS)

Mackintosh, B. H.

1982-01-01

Connection method applies force to two interfaces: that between heating element proper and heating-element support members and between heating-element support members and metal conductor. Inner rod of new connector system is maintained in tension by a spring (for example, Belleville washers). Connection is sufficiently complaint so tension remains within desired range, regardless of thermal expansion and contraction of various elements.

Graphite tail powder and liquid biofertilizer as trace elements source for ground nut

NASA Astrophysics Data System (ADS)

Hindersah, Reginawanti; Setiawati, M. Rochimi; Fitriatin, B. Natalie; Suryatama, Pujawati; Asmiran, Priyanka; Panatarani, Camellia; Joni, I. Made

2018-02-01

Utilization of graphite tail waste from the mineral beneficiation processing is very important since it contain significant amount of essential minerals which are necessary for plant growth. These mineral are required in biochemical processes and mainly play an important role as cofactor in enzymatic reaction. The objective of this research is to investigate the performance of graphite tail on supporting plant growth and yield of ground nut (Arachishypogeae L.). A field experiment has been performed to test the performance of mixed graphite tail and reduced organic matter dose. The graphite tail size were reduced to various sieved size, -80 mesh, -100 mesh and -200 mesh. The experiment was setup in randomized block design with 4 treatments and 6 replications for each treatment, while the control plot is received without graphite tail. The results demonstrated that reduced organic matter along with -200 mesh tail has potentially decreased plant height at the end of vegetative growth stage, in contrast for to -80 mesh tail amendment increased individual fresh plant biomass. Statistically, there was no change of plant nodule, individual shoot fresh and dry weight, root nodule, number of pod following any mesh of graphite tail amendment. Reducing organic matter while adding graphite tail of 5% did not change bean weight in all plot. In contrast, reduced organic matter along with 80-mesh graphite tail amendment improved the nut yield per plot. This experiment suggests that graphite tail, mainly -80 mesh graphite tail can be possibly used in legume production.

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.

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. © 2013 Elsevier B.V. All rights reserved.

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). Copyright © 2014 Elsevier B.V. All rights reserved.

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%).

Metallic impurities-silicon carbide interaction in HTGR fuel particles

NASA Astrophysics Data System (ADS)

Minato, Kazuo; Ogawa, Toru; Kashimura, Satoru; Fukuda, Kousaku; Shimizu, Michio; Tayama, Yoshinobu; Takahashi, Ishio

1990-12-01

Corrosion of the coating layers of silicon carbide (SiC) by metallic impurities was observed in irradiated Triso-coated uranium dioxide particles for high temperature gas-cooled reactors with an optical microscope and an electron probe micro-analyzer. The SiC layers were attacked from the outside of the particles. The main element observed in the corroded areas was iron, but sometimes iron and nickel were found. These elements must have been contained as impurities in the graphite matrix in which the coated particles were dispersed. Since these elements are more stable thermodynamically in the presence of SiC than in the presence of graphite at irradiation temperatures, they were transferred to the SiC layer to form more stable silicides. During fuel manufacturing processes, intensive care should be taken to prevent the fuel from being contaminated with those elements which react with SiC.

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.

Bolted joints in graphite-epoxy composites

NASA Technical Reports Server (NTRS)

Hart-Smith, L. J.

1976-01-01

All-graphite/epoxy laminates and hybrid graphite-glass/epoxy laminates were tested. The tests encompassed a range of geometries for each laminate pattern to cover the three basic failure modes - net section tension failure through the bolt hole, bearing and shearout. Static tensile and compressive loads were applied. A constant bolt diameter of 6.35 mm (0.25 in.) was used in the tests. The interaction of stress concentrations associated with multi-row bolted joints was investigated by testing single- and double-row bolted joints and open-hole specimens in tension. For tension loading, linear interaction was found to exist between the bearing stress reacted at a given bolt hole and the remaining tension stress running by that hole to be reacted elsewhere. The interaction under compressive loading was found to be non-linear. Comparative tests were run using single-lap bolted joints and double-lap joints with pin connection. Both of these joint types exhibited lower strengths than were demonstrated by the corresponding double-lap joints. The analysis methods developed here for single bolt joints are shown to be capable of predicting the behavior of multi-row joints.

Thermal analysis of HGFQ using FIDAP(trademark): Solidification front motion

NASA Technical Reports Server (NTRS)

Woodbury, Keith A.

1996-01-01

The High Gradient Furnace with Quench (HGFQ) is being designed by NASA/MSFC for flight on the International Space Station. The furnace is being designed specifically for solidification experiments in metal and metallic alloy systems. The HGFQ Product development Team (PDT) has been active since January 1994 and their effort is now in early Phase B. Thermal models have been developed both by NASA and Sverdrup (support contractor) to assist in the HGFQ design effort. Both these models use SINDA as a solution engine, but the NASA model was developed using PATRAN and includes more detail than the Sverdrup model. These models have been used to guide design decisions and have been validated through experimentation on a prototypical 'Breadboard' furnace at MSFC. One facet of the furnace operation of interest to the designers is the sensitivity of the solidification interface location to changes in the furnace setpoint. Specifically of interest is the motion (position and velocity) of the solidification front due to a small perturbation in the furnace temperature. FIDAP(TM) is a commercially available finite element program for analysis of heat transfer and fluid flow processes. Its strength is in solution of the Navier-Stokes equations for incompressible flow, but among its capabilities is the analysis of transient processes involving radiation and solidification. The models presently available from NASA and Sverdrup are steady-state models and are incapable of computing the motion of the solidification front. The objective of this investigation is to use FIDAP(TM) to compute the motion of the solidification interface due to a perturbation in the furnace setpoint.

The Effect of Powder Ball Milling on the Microstructure and Mechanical Properties of Sintered Fe-Cr-Mo-Mn-(Cu) Steel

NASA Astrophysics Data System (ADS)

Kulecki, P.; Lichańska, E.

2017-12-01

The effect of ball milling powder mixtures of Höganäs pre-alloyed iron Astaloy CrM, low-carbon ferromanganese Elkem, elemental electrolytic Cu and C-UF graphite on the sintered structure and mechanical properties was evaluated. The mixing was conducted using Turbula mixer for 30 minutes and CDI-EM60 frequency inverter for 1 and 2 hours. Milling was performed on 150 g mixtures with (in weight %) CrM + 1% Mn, CrM + 2% Mn, CrM + 1% Mn + 1% Cu and CrM + 2% Mn + 1% Cu, all with 0.6%C. The green compacts were single pressed at 660 MPa according to PN-EN ISO 2740. Sintering was carried out in a laboratory horizontal furnace Carbolite STF 15/450 at 1250°C for 60 minutes in 5%H2 - 95%N2 atmosphere with a heating rate of 75°C/min, followed by sintering hardening at 60°C/min cooling rate. All the steels were characterized by martensitic structures. Mechanical testing revealed that steels based on milled powders have slightly higher mechanical properties compared to those only mixed and sintered. The best combination of mechanical properties, for ball milled CrM + 1% Mn + 1% Cu was UTS 1046 MPa, TRS 1336 MPa and A 1.94%.

Induced Phytoextraction of Lead Through Chemical Manipulation of Switchgrass and Corn; Role of Iron Supplement.

PubMed

Johnson, Deayne M; Deocampo, Daniel M; El-Mayas, Hanan; Greipsson, Sigurdur

2015-01-01

The effects of combined chemical application of benomyl, ethylenedianinetetraacetate (EDTA), and iron (Fe) (foliar and root) on lead (Pb) phytoextraction by switchgrass (Panicum virgatum) and corn (Zea mays) was examined. Switchgrass was grown in Pb-contaminated urban topsoil with the following treatments: (C) Control, (B) benomyl, (E) EDTA, (F) foliar-Fe, (BE) benomyl + EDTA, (BF) benomyl + foliar-Fe, (FE) foliar-Fe + EDTA, (BFE) benomyl + foliar-Fe + EDTA. Corn was grown in sand-culture supplemented with Pb (500 mg kg(-1)) with the following treatments: (C) control, (B) benomyl, (E) EDTA, (F) root-Fe, (BE) benomyl + EDTA, (BF) benomyl + root-Fe, (FE) root-iron + EDTA, and, (BFE) benomyl + root-Fe + EDTA. All treatments were replicated three times and pots were arranged in a completely randomized design. Plants were analyzed for element concentration (Fe, Zn, P, and Pb) using either inductively coupled plasma (argon) atomic emission spectroscopy (ICP-AES) or graphite furnace atomic absorption spectrometer. Iron supplementation (foliar and root) affected Pb-translocation in plants. Foliar-Fe treatment increased translocation ratio of Pb (TF-Pb) significantly compared to other treatments with the exception of plants treated with benomyl and BF. Root-Fe treatment in combination with EDTA (FE) increased TF-Pb significantly compared to other treatments. Phytoextraction was improved by the combined chemical application; plants treated with BFE treatment increased Pb-total-phytoextraction by 424% compared to Control plants.

Selenium supplementation to chronic kidney disease patients on hemodialysis does not induce the synthesis of plasma glutathione peroxidase.

PubMed

Zachara, Bronislaw A; Gromadzinska, Jolanta; Zbrog, Zbigniew; Swiech, Rafal; Wasowicz, Wojciech; Twardowska, Ewa; Jablonska, Ewa; Sobala, Wojciech

2009-01-01

Numerous authors have shown that selenium (Se) concentration and glutathione peroxidase (GSH-Px) activity in plasma of chronic kidney disease (CKD) patients are lower than in healthy subjects, but there are only few publications on the level of GSH-Px protein in those patients and no reports on the effect of Se supplementation to HD patients on the level of this enzyme. Se concentration and GSH-Px protein level in plasma were measured in a group of 30 CKD patients on hemodialysis (HD) supplemented with 200 microg Se/day for 3 months, and 28 patients on HD administered with placebo. Se concentration was measured by graphite furnace atomic absorption spectrometry and plasma GSH-Px protein level by the sandwich ELISA method using polyclonal antibody specific for human plasma GSH-Px. Se concentration in patients on placebo did not change throughout the 3-month study period, but increased significantly in Se supplemented group. Se supplementation to CKD patients on HD had no effect on the level of GSH-Px protein. The lack of GSH-Px protein in CKD patients on HD is not linked to Se deficiency since the level of this element increased after Se supplementation while enzyme protein level did not change. The damaged kidney of HD patients is unable to synthesize GSH-Px, even after induction with selenium.

Size characterization by Sedimentation Field Flow Fractionation of silica particles used as food additives.

PubMed

Contado, Catia; Ravani, Laura; Passarella, Martina

2013-07-25

Four types of SiO2, available on the market as additives in food and personal care products, were size characterized using Sedimentation Field Flow Fractionation (SdFFF), SEM, TEM and Photon Correlation Spectroscopy (PCS). The synergic use of the different analytical techniques made it possible, for some samples, to confirm the presence of primary nanoparticles (10 nm) organized in clusters or aggregates of different dimension and, for others, to discover that the available information is incomplete, particularly that regarding the presence of small particles. A protocol to extract the silica particles from a simple food matrix was set up, enriching (0.25%, w w(-1)) a nearly silica-free instant barley coffee powder with a known SiO2 sample. The SdFFF technique, in conjunction with SEM observations, made it possible to identify the added SiO2 particles and verify the new particle size distribution. The SiO2 content of different powdered foodstuffs was determined by graphite furnace atomic absorption spectroscopy (GFAAS); the concentrations ranged between 0.006 and 0.35% (w w(-1)). The protocol to isolate the silica particles was so applied to the most SiO2-rich commercial products and the derived suspensions were separated by SdFFF; SEM and TEM observations supported the size analyses while GFAAS determinations on collected fractions permitted element identification. Copyright © 2013 Elsevier B.V. All rights reserved.

Breathing of Graphite Particles in a Lithium-Ion Battery

NASA Astrophysics Data System (ADS)

Takata, Keiji; Okuda, Mitsuhiro; Yura, Nobuki; Tamura, Ryota

2012-04-01

We imaged changes in volume of graphite particles in a Li-ion battery due to the insertion and extraction of Li ions using scanning probe microscopy. When Li ions were extracted from the graphite particles, the particles were contracted, while expansion was induced in the interspaces between the particles. Variations of the images of volume changes depending on modulation frequencies clearly showed lithium intercalation. A linear relationship between the amplitudes of volume changes and the products of the diffusion elements and the reciprocals of the frequencies has been proven. Thus, the detected signals quantitatively well corresponded to the lithium ion movements.

Release of Si from Silicon, a Ferrosilicon (FeSi) Alloy and a Synthetic Silicate Mineral in Simulated Biological Media

PubMed Central

Herting, Gunilla; Jiang, Tao; Sjöstedt, Carin; Odnevall Wallinder, Inger

2014-01-01

Unique quantitative bioaccessibility data has been generated, and the influence of surface/material and test media characteristics on the elemental release process were assessed for silicon containing materials in specific synthetic body fluids at certain time periods at a fixed loading. The metal release test protocol, elaborated by the KTH team, has previously been used for classification, ranking, and screening of different alloys and metals. Time resolved elemental release of Si, Fe and Al from particles, sized less than 50 µm, of two grades of metallurgical silicon (high purity silicon, SiHG, low purity silicon, SiLG), an alloy (ferrosilicon, FeSi) and a mineral (aluminium silicate, AlSi) has been investigated in synthetic body fluids of varying pH, composition and complexation capacity, simple models of for example dermal contact and digestion scenarios. Individual methods for analysis of released Si (as silicic acid, Si(OH)4) in synthetic body fluids using GF-AAS were developed for each fluid including optimisation of solution pH and graphite furnace parameters. The release of Si from the two metallurgical silicon grades was strongly dependent on both pH and media composition with the highest release in pH neutral media. No similar effect was observed for the FeSi alloy or the aluminium silicate mineral. Surface adsorption of phosphate and lactic acid were believed to hinder the release of Si whereas the presence of citric acid enhanced the release as a result of surface complexation. An increased presence of Al and Fe in the material (low purity metalloid, alloy or mineral) resulted in a reduced release of Si in pH neutral media. The release of Si was enhanced for all materials with Al at their outermost surface in acetic media. PMID:25225879

Solar Tests of Aperture Plate Materials for Solar Thermal Dish Collectors

NASA Technical Reports Server (NTRS)

Jaffe, L. D.

1984-01-01

If a malfunction occurs in a solar thermal point-focus distributed receiver power plant while a concentrator is pointed at the Sun, motion of the concentrator may stop. As the Sun moves relative to the Earth, the spot of concentrated sunlight then slowly walks off the receiver aperture, across the receiver face plate, and perhaps across adjacent portions of the concentrator. Intense local heating by the concentrated sunlight may damage or destroy these parts. The behavior of various materials under conditions simulating walk-off of a parabolic dish solar collector were evaluated. Each test consisted of exposure to concentrated sunlight at a peak flux density of about 7000 kW/square meter for 15 minutes. Types of materials tested included graphite, silicon carbide, silica, various silicates, alumina, zirconia, aluminum, copper, steel, and polytetrafluoroethylene. The only material that neither cracked nor melted was grade G-90 graphite. Grade CS graphite, a lower cost commercial grade, cracked half-way across, but did not fall apart. Both of these grades are medium-grain extruded graphites. A graphite cloth (graphitized polyacrylonitrile) showed fair performance when tested as a single thin ply; it might be useful as a multi-ply assembly. High purity slipcast silica showed some promise also.

Solar tests of aperture plate materials for solar thermal dish collectors

NASA Technical Reports Server (NTRS)

Jaffe, L. D.

1984-01-01

If a malfunction occurs in a solar thermal point-focus distributed receiver power plant while a concentrator is pointed at the sun, motion of the concentrator may stop. As the sun moves relative to the earth, the spot of concentrated sunlight then slowly walks off the receiver aperture, across the receiver face plate, and perhaps across adjacent portions of the concentrator. Intense local heating by the concentrated sunlight may damage or destroy these parts. The behavior of various materials under conditions simulating walk-off of a parabolic dish solar collector were evaluated. Each test consisted of exposure to concentrated sunlight at a peak flux density of about 7000 kW/square meter for 15 minutes. Types of materials tested included graphite, silicon carbide, silica, various silicates, alumina, zirconia, aluminum, copper, steel, and polytetrafluroethylene. The only material that neither cracked nor melted was grade G-90 graphite. Grade CS graphite, a lower cost commercial grade, cracked half-way across, but did not fail apart. Both of these grades are medium-grain extruded graphites. A graphite cloth (graphitized polyacrylonitrile) showed fair performance when tested as a single thin ply; it might be useful as a multi-ply assembly. High purity slipcast silica showed some promise also.

Solar tests of aperture plate materials for solar thermal dish collectors

NASA Technical Reports Server (NTRS)

Jaffe, L. D.

1984-01-01

If a malfunction occurs in a solar thermal point-focus distributed receiver power plant while a concentrator is pointed at the sun, motion of the concentrator may stop. As the sun moves relative to the earth, the spot of concentrated sunlight then slowly walks off the receiver aperture, across the receiver face plate, and perhaps across adjacent portions of the concentrator. Intense local heating by the concentrated sunlight may damage or destroy these parts. The behavior of various materials under conditions simulating walk-off of a parabolic dish solar collector were evaluated. Each test consisted of exposure to concentrated sunlight at a peak flux density of about 7000 kW/square meter for 15 minutes. Types of materials tested included graphite, silicon carbide, silica, various silicates, alumina, zirconia, aluminum, copper, steel, and polytetrafluoroethylene. The only material that neither cracked nor melted was grade G-90 graphite. Grade CS graphite, a lower cost commercial grade, cracked half-way across, but did not fall apart. Both of these grades are medium-grain extruded graphites. A graphite cloth (graphitized polyacrylonitrile) showed fair performance when tested as a single thin ply; it might be useful as a multi-ply assembly. High purity slipcast silica showed some promise also.

Vaporization thermodynamics of K2S and K2SO3

NASA Technical Reports Server (NTRS)

Bennet, J. E.

1982-01-01

The vaporization reactions, vapor pressures, and thermodynamics of potassium sulfide and potassium sulfite were studied for purposes of providing fundamental data for the seed cycle in magnetohydrodynamic electric power generation. Rate of effusion studies, supported by tube furnace experiments, X-ray powder diffraction, mass spectrometry and appropriate chemical analyses and tests, revealed that potassium sulfite disproportionates at high temperatures to form potassium sulfide and potassium sulfate. Potassium sulfide was observed to vaporize incongruently, the initial vapors beng predominantly potassium atoms, with minor species being S2 and various K-S molecules. The ratio of K/S2 in the vapor is very large initially and decreases steadily with prolonged heating. Several materials were evaluated for purposes of containing K2S/K2SO3 at temperatures or = 800 C: Pt, Mo, W, quartz, machinable glass, BN, high density graphite, pyrolytic coated graphite, and alumina. Of these, only alumina was observed to be chemically inert to both K2S but reacted with K2SO3. The other materials were not suitable for either substance. Thermodynamic calculations based on measured vapor pressures and approximate free energy functions are described. Results from isothermal total mass loss experiments and from thermogravimetric experiments are also included.

Adsorption of Paraquat Dichloride by Graphitic Carbon Nitride Synthesized from Melamine Scraps

NASA Astrophysics Data System (ADS)

Watcharenwong, A.; Kaeokan, A.; Rammaroeng, R.; Upama, P.; Kajitvichyanukul, P.

2017-07-01

In this research, graphitic carbon nitride (g-C3N4) was synthesized from useless melamine scraps. Mixture of melamine powder and urea was directly burned in the muffle furnace at 550 °C. Later as-synthesized g-C3N4 was modified with hydrochloric acid. The g-C3N4 powder was characterized by several techniques including X-ray diffraction, scanning electron microscope, and specific surface area analyser. Adsorption of the herbicide paraquat from an aqueous solution to suspended particles of g-C3N4 was investigated, taking into consideration several parameters such as initial concentration of paraquat, initial pH, and dosage of g-C3N4. The results showed that with the same amount of g-C3N4, the increase in the paraquat concentration caused the reduction in the removal efficiency and the higher the amount of g-C3N4, the less residual paraquat remained in the bulk solution. G-C3N4 showed better adsorption behaviour in the basic condition. Finally, Langmuir and Freundlich adsorption isotherms were also evaluated. Paraquat adsorption by g-C3N4 was in accordance with Langmuir more than Freundlich adsorption isotherm.

Brazed graphite/refractory metal composites for first-wall protection elements

NASA Astrophysics Data System (ADS)

Šmid, I.; Croessmann, C. D.; Salmonson, J. C.; Whitley, J. B.; Kny, E.; Reheis, N.; Kneringer, G.; Nickel, H.

1991-03-01

The peak surface heat flux deposition on divertor elements of near term fusion devices is expected to exceed 10 MW/m 2. The needed reliability of brazed plasma interactive components, particularly under abnormal operating conditions with peak surface temperatures well beyond 1000°C, makes refractory metallic substrates and brazes with a high melting point very attractive. TZM, a high temperature alloy of molybdenum, and isotropic graphite, materials very closely matched in their thermal expansion, were brazed with four high-temperature brazes. The brazes used were Zr, 90Ni/10Ti, 90Cu/10Ti and 70Ag/27Cu/3Ti (nominal composition prior to brazing, wt%). The resulting composite tiles of 50 × 50 mm2 with a TZM thickness of 5 mm and a graphite thickness of 10 mm have been tested in high heat flux simulation for their thermal fatigue properties. Up to 600 loading cycles were carried out with an average heat flux of 10 MW/m 2 for 0.5 s pulses. The maximum surface temperature was 1100°C. In support of the experiment, the thermal response and temperature gradients of the samples were investigated using a finite element model.

The effect of carbon crystal structure on treat reactor physics calculations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Swanson, R.W.; Harrison, L.J.

1988-01-01

The Transient Reactor Test Facility (TREAT) at Argonne National Laboratory-West (ANL-W) is fueled with urania in a graphite and carbon mixture. This fuel was fabricated from a mixture of graphite flour, thermax (a thermatomic carbon produced by ''cracking'' natural gas), coal-tar resin and U/sub 3/O/sub 8/. During the fabrication process, the fuel was baked to dissociate the resin, but the high temperature necessary to graphitize the carbon in the thermax and in the resin was avoided. Therefore, the carbon crystal structure is a complex mixture of graphite particles in a nongraphitized elemental carbon matrix. Results of calculations using macroscopic carbonmore » cross sections obtained by mixing bound-kernel graphite cross sections for the graphitized carbon and free-gas carbon cross sections for the remainder of the carbon and calculations using only bound-kernel graphite cross sections are compared to experimental data. It is shown that the use of the hybridized cross sections which reflect the allotropic mixture of the carbon in the TREAT fuel results in a significant improvement in the accuracy of calculated neutronics parameters for the TREAT reactor. 6 refs., 2 figs., 3 tabs.« less

Evaluation on chemical stability of lead blast furnace (LBF) and imperial smelting furnace (ISF) slags.

PubMed

Yin, Nang-Htay; Sivry, Yann; Guyot, François; Lens, Piet N L; van Hullebusch, Eric D

2016-09-15

The leaching behavior of Pb and Zn from lead blast furnace (LBF) and imperial smelting furnace (ISF) slags sampled in the North of France was studied as a function of pHs and under two atmospheres (open air and nitrogen). The leaching of major elements from the slags was monitored as a function of pH (4, 5.5, 7, 8.5 and 10) under both atmospheres for different slag-water interaction times (1 day and 9 days). The leaching results were coupled with a geochemical model; Visual MINTEQ version 3.0, and a detailed morphological and mineralogical analysis was performed on the leached slags by scanning and transmission electron microscopy (SEM and TEM). Significant amounts of Ca, Fe and Zn were released under acidic conditions (pH 4) with a decrease towards the neutral to alkaline conditions (pH 7 and 10) for both LBF and ISF slags. On the other hand, Fe leachability was limited at neutral to alkaline pH for both slags. The concentrations of all elements increased gradually after 216 h compared to initial 24 h of leaching period. The presence of oxygen under open-air atmosphere not only enhanced oxidative weathering but also encouraged formation of secondary oxide and carbonate phases. Formation of carbonates and clay minerals was suggested by Visual MINTEQ which was further confirmed by SEM & TEM. The hydration and partial dissolution of hardystonite, as well as the destabilization of amorphous glassy matrix mainly contributed to the release of major elements, whereas the spinel related oxides were resistant against pH changes and atmospheres within the time frame concerned for both LBF and ISF slags. The total amount of Pb leached out at pH 7 under both atmospheres suggested that both LBF and ISF slags are prone to weathering even at neutral environmental conditions. Copyright © 2016 Elsevier Ltd. All rights reserved.

A COOLED NEUTRONIC REACTOR

DOEpatents

Wigner, E.P.; Creutz, E.C.

1960-03-15

A nuclear reactor comprising a pair of graphite blocks separated by an air gap is described. Each of the blocks contains a plurality of channels extending from the gap through the block with a plurality of fuel elements being located in the channels. Means are provided for introducing air into the gap between the graphite blocks and for exhausting the air from the ends of the channels opposite the gap.

Intelligent Support System of Steel Technical Preparation in an Arc Furnace: Functional Scheme of Interactive Builder of the Multi Objective Optimization Problem

NASA Astrophysics Data System (ADS)

Logunova, O. S.; Sibileva, N. S.

2017-12-01

The purpose of the study is to increase the efficiency of the steelmaking process in large capacity arc furnace on the basis of implementation a new decision-making system about the composition of charge materials. The authors proposed an interactive builder for the formation of the optimization problem, taking into account the requirements of the customer, normative documents and stocks of charge materials in the warehouse. To implement the interactive builder, the sets of deterministic and stochastic model components are developed, as well as a list of preferences of criteria and constraints.

Microgravity Disturbance Characterization of the Quench Module Insert (QMI) Phase Change Device (PCD)

NASA Technical Reports Server (NTRS)

Gattis, Christy; Rodriguez, Pete (Technical Monitor)

2000-01-01

The Materials Science Research Facility (MSRF) is a multi-user, multi-purpose facility for materials science research. One experiment within the MSRF will be the Quench Module Insert (QMI), a high-temperature furnace with unique capabilities for processing different classes of materials. The primary functions of the QMI furnace are to melt, directionally solidify, and quench metallic samples, providing data to aid in understanding the effects of the microgravity environment on the characteristics of these processed metals. The QMI houses sealed individual sample ampoules containing material to be processed. Quenching of the samples in the QMI furnace is accomplished by releasing low-melting-point metallic shoes into contact with the outside of the sample ampoule, dissipating heat and cooling the sample inside. The impact from this method of quench will induce sample vibrations which could be large enough to adversely affect sample quality. Utilizing breadboard hardware, the sample quench sequence, releasing the shoes, was conducted. Data was collected from accelerometers located on the breadboard sample cartridge, indicating the maximum acceleration achieved by the sample. The primary objective of the test described in this presentation was to determine the acceleration imparted on the sample by the shoe contact. From this information, the science community can better assess whether this method of quench will allow them to obtain the data they need.

Investigation of Conditions of Titanium Carbonization - IV

NASA Technical Reports Server (NTRS)

Meerson, G. A.; Lipkes, Y. M.

1949-01-01

In a previous paper, results are presented of accurate investigations of the processes of titanium carbonization and the succeeding titanium carbide decarbonization as related to the phenomenon of the graphitization of soot by heating at a constant temperature in atmospheres of pure hydrogen and carbon monoxide. These tests showed that the processes of titanium carbonization-decarbonization in an atmosphere of pure gases without nitrogen proceed in the same direction as the analogous processes under the conditions of the production furnace. In this case, however, the presence of admixtures of nitrogen changes the quantitative results of the decarbonization process. Thermodynamic computations confirming the results of previous tests conducted at atmospheric pressure and additional tests of titanium carbonization at lowered pressures are presented herein.

Pollution in acid mine drainage from mine tailings in Svalbard Norwegian Arctic

NASA Astrophysics Data System (ADS)

Holm, E. B.; Brandvik, P. J.; Steinnes, E.

2003-05-01

Throughout the summer season of 2000 samples of acid mine drainage (AMD) were collected from areas below tailing deposits from the coal mining in Svalbard, Norwegian Arctic. The water was analysed for pH, oxygen, conductivity, 9 sulfate and various metals. Oxygen, pH and conductivity were measured by standard electrodes, sulphate was determined gravimetrically and metals were determined by flame/graphite furnace AAS. The AMD was found to contain heavy metals and sulphate in high concentrations, causing damage to the local tundra vegetation. Large spatial variation however was observed in pH (2.5-9.5) as well as in metal concentrations in the AMD, indicating strongly inhomogeneous distribution of sulphide minerais in the tailing deposits.

Considerations in As analysis and speciation

USGS Publications Warehouse

Edwards, M.; Patel, S.; McNeil, L.; Chen, H.W.; Frey, M.; Eaton, A.D.; Antweiler, Ronald C.; Taylor, Howard E.

1998-01-01

This article summarizes recent experiences in arsenic (As) quantification, preservation, and speciation developed during AWWA Research Foundation (AWWARF) and Water Industry Technical Action Fund (WITAF) projects. The goal of this article is to alert analysts and decision-makers to potential problems in As analysis and speciation, because there appear to be several unresolved problems with routine analytical approaches. In true split drinking water samples As was quantified by three accepted analytical methods in three laboratories. The techniques used were graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma mass spectrometry (ICP-MS), and hydride generation inductively coupled plasma-emission spectrometry (HG-ICP-AES). Experimental findings are organized into sections on As analysis, particulate As in water supplies, and examination of As speciation methods.

Blood lead levels and risk factors in pregnant women from Durango, Mexico.

PubMed

La-Llave-León, Osmel; Estrada-Martínez, Sergio; Manuel Salas-Pacheco, José; Peña-Elósegui, Rocío; Duarte-Sustaita, Jaime; Candelas Rangel, Jorge-Luís; García Vargas, Gonzalo

2011-01-01

In this cross-sectional study the authors determined blood lead levels (BLLs) and some risk factors for lead exposure in pregnant women. Two hundred ninety-nine pregnant women receiving medical attention by the Secretary of Health, State of Durango, Mexico, participated in this study between 2007 and 2008. BLLs were evaluated with graphite furnace atomic absorption spectrometry. The authors used Student t test, 1-way analysis of variance (ANOVA), and linear regression as statistical treatments. BLLs ranged from 0.36 to 23.6 μg/dL (mean = 2.79 μg/dL, standard deviation = 2.14). Multivariate analysis showed that the main predictors of BLLs were working in a place where lead is used, using lead glazed pottery, and eating soil.

Hot wire production of single-wall and multi-wall carbon nanotubes

DOEpatents

Dillon, Anne C.; Mahan, Archie H.; Alleman, Jeffrey L.

2010-10-26

Apparatus (210) for producing a multi-wall carbon nanotube (213) may comprise a process chamber (216), a furnace (217) operatively associated with the process chamber (216), and at least one filament (218) positioned within the process chamber (216). At least one power supply (220) operatively associated with the at least one filament (218) heats the at least one filament (218) to a process temperature. A gaseous carbon precursor material (214) operatively associated with the process chamber (216) provides carbon for forming the multi-wall carbon nanotube (213). A metal catalyst material (224) operatively associated with the process (216) catalyzes the formation of the multi-wall carbon nanotube (213).

Carbon or graphite foam as a heating element and system thereof

DOEpatents

Ott, Ronald D [Knoxville, TN; McMillan, April D [Knoxville, TN; Choudhury, Ashok [Oak Ridge, TN

2004-05-04

A temperature regulator includes at least one electrically conductive carbon foam element. The foam element includes at least two locations adapted for receiving electrical connectors thereto for heating a fluid, such as engine oil. A combustion engine includes an engine block and at least one carbon foam element, the foam element extending into the engine block or disposed in thermal contact with at least one engine fluid.

Global transport of light elements boron and carbon in the full-W ASDEX Upgrade

NASA Astrophysics Data System (ADS)

ASDEX Upgrade Team; Hakola, A.; Likonen, J.; Koivuranta, S.; Krieger, K.; Mayer, M.; Neu, R.; Rohde, V.; Sugiyama, K.

2011-08-01

Transport of carbon and boron has been investigated in the full-W ASDEX Upgrade after experimental campaigns with (2008) and without (2007) boronizations. For this purpose, poloidal deposition profiles of the two elements on tungsten and graphite regions of lower-divertor tiles have been determined. Carbon is mainly deposited in the inner divertor - 80-90% of the determined 12C and 13C inventories on W - while boron shows a much more symmetric deposition profile. In the unboronized machine, the boron inventories are a factor of 10 smaller than in the boronized case and result from residual boron atoms left in the torus prior to the 2007 campaign. Both carbon and boron are deposited more efficiently and/or show less erosion on graphite than on tungsten, particularly in the outer divertor. For 13C, the difference is 10-100 in favor of graphite. This is most probably caused by a higher re-erosion from tungsten surfaces.

Systems integration and demonstration of advanced reusable structure for ALS

NASA Technical Reports Server (NTRS)

Gibbins, Martin N.

1991-01-01

The objective was to investigate the potential of advanced material to achieve life cycle cost (LCC) benefits for reusable structure on the advanced launch system. Three structural elements were investigated - all components of an Advanced Launch System reusable propulsion/avionics module. Leading aeroshell configurations included sandwich structure using titanium, graphite/polyimide (Gr/PI), or high-temperature aluminum (HTA) face sheets. Thrust structure truss concepts used titanium, graphite/epoxy, or silicon carbide/aluminum struts. Leading aft bulkhead concepts employed graphite epoxy and aluminum. The technical effort focused on the aeroshell because the greatest benefits were expected there. Thermal analyses show the structural temperature profiles during operation. Finite element analyses show stresses during splash-down. Weight statements and manufacturing cost estimates were prepared for calculation of LCC for each design. The Gr/PI aeroshell showed the lowest potential LCC, but the HTA aeroshell was judged to be lower risk. A technology development plan was prepared to validate the applicable structural technology.

SIKA—the multiplexing cold-neutron triple-axis spectrometer at ANSTO

NASA Astrophysics Data System (ADS)

Wu, C.-M.; Deng, G.; Gardner, J. S.; Vorderwisch, P.; Li, W.-H.; Yano, S.; Peng, J.-C.; Imamovic, E.

2016-10-01

SIKA is a new cold-neutron triple-axis spectrometer receiving neutrons from the cold source CG4 of the 20MW Open Pool Australian Light-water reactor. As a state-of-the-art triple-axis spectrometer, SIKA is equipped with a large double-focusing pyrolytic graphite monochromator, a multiblade pyrolytic graphite analyser and a multi-detector system. In this paper, we present the design, functions, and capabilities of SIKA, and discuss commissioning experimental results from powder and single-crystal samples to demonstrate its performance.

Research Report to the National Aeronautics and Space Administration Cosmochemistry Program

NASA Technical Reports Server (NTRS)

Alexander, Conel O'D.

2004-01-01

The discovery of presolar grains in meteorites is one of the most exciting recent developments in meteoritics. Six types of presolar grain have been discovered: diamond, Sic, graphite, Si3N4, Al2O3 and MgAl2O4 (NIITLER, 2003). These grains have been identified as presolar because their isotopic compositions are very different from those of Solar System materials. Comparison of their isotopic compositions with astronomical observations and theoretical models indicates that most of the grains formed in the envelopes of highly evolved stars. They are, therefore, a new source of information with which to test astrophysical models of the evolution of these stars. In fact, because several elements can often be measured in the same grain, including elements that are not measurable spectroscopically in stars, the grain data provide some very stringent constraints for these models. Our primary goal is to create large, unbiased, multi-isotope databases of single presolar Sic, Si3N4, oxide and graphite grains in meteorites, as well as any new presolar grain types that are identified in the future. These will be used to: (i) test stellar and nucleosynthetic models, (ii) constrain the galactic chemical evolution (GCE) paths of the isotopes of Si, Ti, O and Mg, (iii) establish how many stellar sources contributed to the Solar System, (iv) constrain relative dust production rates of various stellar types and (v) assess how representative of galactic dust production the record in meteorites is. The primary tool for this project is a highly automated grain analysis system on the Carnegie 6f ion probe. This proposal was part of a long-standing research effort that is still ongoing.

Optimal Recycling of Steel Scrap and Alloying Elements: Input-Output based Linear Programming Method with Its Application to End-of-Life Vehicles in Japan.

PubMed

Ohno, Hajime; Matsubae, Kazuyo; Nakajima, Kenichi; Kondo, Yasushi; Nakamura, Shinichiro; Fukushima, Yasuhiro; Nagasaka, Tetsuya

2017-11-21

Importance of end-of-life vehicles (ELVs) as an urban mine is expected to grow, as more people in developing countries are experiencing increased standards of living, while the automobiles are increasingly made using high-quality materials to meet stricter environmental and safety requirements. While most materials in ELVs, particularly steel, have been recycled at high rates, quality issues have not been adequately addressed due to the complex use of automobile materials, leading to considerable losses of valuable alloying elements. This study highlights the maximal potential of quality-oriented recycling of ELV steel, by exploring the utilization methods of scrap, sorted by parts, to produce electric-arc-furnace-based crude alloy steel with minimal losses of alloying elements. Using linear programming on the case of Japanese economy in 2005, we found that adoption of parts-based scrap sorting could result in the recovery of around 94-98% of the alloying elements occurring in parts scrap (manganese, chromium, nickel, and molybdenum), which may replace 10% of the virgin sources in electric arc furnace-based crude alloy steel production.

Use of graphite epoxy composites in the Solar-A Soft X-Ray Telescope

NASA Technical Reports Server (NTRS)

Jurcevich, B. K.; Bruner, M. E.

1990-01-01

This paper describes the use of composite materials in the Soft X-Ray Telescope (SXT). One of the primary structural members of the telescope is a graphite epoxy metering tube. The metering tube maintains the structural stability of the telescope during launch as well as the focal length through various environmental conditions. The graphite epoxy metering tube is designed to have a negative coefficient of thermal expansion to compensate for the positive expansion of titanium structural supports. The focus is maintained to + or - 0.001 inch by matching the CTE of the composite tube to the remaining structural elements.

Thermo-viscoelastic response of graphite/epoxy composites

NASA Technical Reports Server (NTRS)

Lin, Kuen; Hwang, I. H.

1988-01-01

The thermo-viscoelastic behavior of composite material is studied analytically using a special finite-element formulation. Numerical results on stress and deformation histories are obtained for both unnotched and notched graphite/epoxy composites subjected to mechanical and thermal spectrum loads. The results indicate that time-dependent effects are important in composites with matrix-dominated layup orientations. Such effects also strongly depend on the specific environment condition and load spectrum applied.

Integration of uncooled scraper elements and its diagnostics into Wendelstein 7-X

DOE PAGES

Fellinger, Joris; Loesser, Doug; Neilson, Hutch; ...

2017-08-08

The modular stellarator Wendelstein 7-X in Greifswald (Germany) successfully started operation in 2015 with short pulse limiter plasmas. In 2017, the next operation phase (OP) OP1.2 will start once 10 uncooled test divertor units (TDU) with graphite armor will be installed. The TDUs allow for plasma pulses of 10 s with 8 MW heating. OP2, allowing for steady state operation, is planned for 2020 after the TDUs will be replaced by 10 water cooled CFC armored divertors. Due to the development of plasma currents like bootstrap currents in long pulse plasmas in OP2, the plasma could hit the edge ofmore » the divertor targets which has a reduced cooling capacity compared to the central part of the target tiles. To prevent overloading of these edges, a so-called scraper element can be positioned in front of the divertor, intersecting those strike lines that would otherwise hit the divertor edges. As a result, these edges are protected but as a drawback the pumping efficiency of neutrals is also reduced. As a test an uncooled scraper element with graphite tiles will be placed in two out of ten half modules in OP1.2. A decision to install ten water cooled scraper elements for OP2 is pending on the results of this test in OP1.2. To monitor the impact of the scraper element on the plasma, Langmuir probes are integrated in the plasma facing surface, and a neutral gas manometer measures the neutral density directly behind the plasma facing surface. Moreover, IR and VIS cameras observe the plasma facing surface and thermocouples monitor the temperatures of the graphite tiles and underlying support structure. This paper describes the integration of the scraper element and its diagnostics in Wendelstein 7-X.« less

MOLDED SEALING ELEMENT

DOEpatents

Bradford, B.W.; Skinner, W.J.

1959-03-24

Molded sealing elements suitable for use under conditions involving exposure to uranium hexafluoride vapor are described. Such sealing elements are made by subjecting graphitic carbons to a preliminary treatment with uranium hexafluoride vapor, and then incorporating polytetrafluorethylene in them. The resulting composition has good wear resistant and frictional properties and is resistant to disintegration by uranium hexafluoride over long periods of exposure.

Purification and preparation of graphite oxide from natural graphite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Panatarani, C., E-mail: c.panatarani@phys.unpad.ac.id; Muthahhari, N.; Joni, I. Made

2016-03-11

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

Towards the development of high temperature comparison artifacts for radiation thermometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Teixeira, R. N.; Machin, G.; Orlando, A.

This paper describes the methodology and first results of the development of high temperature fixed point artifacts of unknown temperature suitable for scale comparison purposes. This study is being undertaken at the Thermal Metrology Division of Inmetro, Brazil, as part of PhD studies. In this initial phase of the study two identical cobalt carbon eutectic cells were constructed and one doped with a known amount of copper. This was an attempt to achieve a controlled change in the transition temperature of the alloy during melting. Copper was chosen due to the relatively simple phase diagram it forms with carbon andmore » cobalt. The cobalt, in powder form, was supplied by Alfa Aesar at 99.998 % purity, and was mixed with carbon powder (1,9 % by weight) of 99.9999 % purity. Complete filling of the crucible took 6 steps and was performed in a vertical furnace with graphite heating elements, in an inert gas atmosphere. The temperature measurements were performed using a KE LP3 radiation thermometer, which was previously evaluated for spectral responsivity, linearity and size-of-source effect (SSE). During these measurements, the thermometer stability was periodically checked using a silver fixed point blackbody maintained in a three zone furnace. The main purpose of the first part of this study is to dope a series of Co-C blackbody with differing amounts of copper, in order to alter their temperatures whilst still retaining good melting plateau performance. The long-term stability of the adjusted transition temperatures will also be investigated. Other dopants will be studied as the research progresses, and thermo chemical modeling will be performed in an attempt to understand the change in temperature with dopant concentration and so help select suitable dopants in the future. The overall objective is to construct comparison artifacts that have good performance, in terms of plateau shape and long-term temperature stability, but with unknown temperatures. These can then be used as comparison artifacts with no participant, except the pilot, knowing the temperature a priori.« less

Discrete element simulation of charging and mixed layer formation in the ironmaking blast furnace

NASA Astrophysics Data System (ADS)

Mitra, Tamoghna; Saxén, Henrik

2016-11-01

The burden distribution in the ironmaking blast furnace plays an important role for the operation as it affects the gas flow distribution, heat and mass transfer, and chemical reactions in the shaft. This work studies certain aspects of burden distribution by small-scale experiments and numerical simulation by the discrete element method (DEM). Particular attention is focused on the complex layer-formation process and the problems associated with estimating the burden layer distribution by burden profile measurements. The formation of mixed layers is studied, and a computational method for estimating the extent of the mixed layer, as well as its voidage, is proposed and applied on the results of the DEM simulations. In studying a charging program and its resulting burden distribution, the mixed layers of coke and pellets were found to show lower voidage than the individual burden layers. The dynamic evolution of the mixed layer during the charging process is also analyzed. The results of the study can be used to gain deeper insight into the complex charging process of the blast furnace, which is useful in the design of new charging programs and for mathematical models that do not consider the full behavior of the particles in the burden layers.

Analysis of characteristics of Si in blast furnace pig iron and calibration methods in the detection by laser-induced breakdown spectroscopy

NASA Astrophysics Data System (ADS)

Mei, Yaguang; Cheng, Yuxin; Cheng, Shusen; Hao, Zhongqi; Guo, Lianbo; Li, Xiangyou; Zeng, Xiaoyan

2017-10-01

During the iron-making process in blast furnace, the Si content in liquid pig iron was usually used to evaluate the quality of liquid iron and thermal state of blast furnace. None effective method was found for rapid detecting the Si concentration of liquid iron. Laser-induced breakdown spectroscopy (LIBS) is a kind of atomic emission spectrometry technology based on laser ablation. Its obvious advantage is realizing rapid, in-situ, online analysis of element concentration in open air without sample pretreatment. The characteristics of Si in liquid iron were analyzed from the aspect of thermodynamic theory and metallurgical technology. The relationship between Si and C, Mn, S, P or other alloy elements were revealed based on thermodynamic calculation. Subsequently, LIBS was applied on rapid detection of Si of pig iron in this work. During LIBS detection process, several groups of standard pig iron samples were employed in this work to calibrate the Si content in pig iron. The calibration methods including linear, quadratic and cubic internal standard calibration, multivariate linear calibration and partial least squares (PLS) were compared with each other. It revealed that the PLS improved by normalization was the best calibration method for Si detection by LIBS.

Rapid analysis method for the determination of 14C specific activity in irradiated graphite

PubMed Central

Remeikis, Vidmantas; Lagzdina, Elena; Garbaras, Andrius; Gudelis, Arūnas; Garankin, Jevgenij; Juodis, Laurynas; Duškesas, Grigorijus; Lingis, Danielius; Abdulajev, Vladimir; Plukis, Artūras

2018-01-01

14C is one of the limiting radionuclides used in the categorization of radioactive graphite waste; this categorization is crucial in selecting the appropriate graphite treatment/disposal method. We propose a rapid analysis method for 14C specific activity determination in small graphite samples in the 1–100 μg range. The method applies an oxidation procedure to the sample, which extracts 14C from the different carbonaceous matrices in a controlled manner. Because this method enables fast online measurement and 14C specific activity evaluation, it can be especially useful for characterizing 14C in irradiated graphite when dismantling graphite moderator and reflector parts, or when sorting radioactive graphite waste from decommissioned nuclear power plants. The proposed rapid method is based on graphite combustion and the subsequent measurement of both CO2 and 14C, using a commercial elemental analyser and the semiconductor detector, respectively. The method was verified using the liquid scintillation counting (LSC) technique. The uncertainty of this rapid method is within the acceptable range for radioactive waste characterization purposes. The 14C specific activity determination procedure proposed in this study takes approximately ten minutes, comparing favorably to the more complicated and time consuming LSC method. This method can be potentially used to radiologically characterize radioactive waste or used in biomedical applications when dealing with the specific activity determination of 14C in the sample. PMID:29370233

Synthesis and characterization of SiC based composite materials for immobilizing radioactive graphite

NASA Astrophysics Data System (ADS)

Wang, Qing; Teng, Yuancheng; Wu, Lang; Zhang, Kuibao; Zhao, Xiaofeng; Hu, Zhuang

2018-06-01

In order to immobilize high-level radioactive graphite, silicon carbide based composite materials{ (1-x) SiC· x MgAl2O4 (0.1 ≤ x≤0.4) } were fabricated by solid-state reaction at 1370 °C for 2 h in vacuum. Residual graphite and precipitated corundum were observed in the as-synthesized product, which attributed to the interface reaction of element silicon and magnesium compounds. To further understand the reasons for the presence of graphite and corundum, the effects of mole ratio of Si/C, MgAl2O4 content and non-stoichiometry of MgAl2O4 on the synthesis were investigated. To immobilize graphite better, residual graphite should be eliminated. The target product was obtained when the mole ratio of Si/C was 1.3:1, MgAl2O4 content was x = 0.2, and the mole ratio of Al to Mg in non-stoichiometric MgAl2O4 was 1.7:1. In addition, the interface reaction between magnesium compounds and silicon not graphite was displayed by conducting a series of comparative experiments. The key factor for the occurrence of interface reaction is that oxygen atom is transferred from magnesium compound to SiO gas. Infrared and Raman spectrum revealed the increased disorders of graphite after being synthesized.

Rapid analysis method for the determination of 14C specific activity in irradiated graphite.

PubMed

Remeikis, Vidmantas; Lagzdina, Elena; Garbaras, Andrius; Gudelis, Arūnas; Garankin, Jevgenij; Plukienė, Rita; Juodis, Laurynas; Duškesas, Grigorijus; Lingis, Danielius; Abdulajev, Vladimir; Plukis, Artūras

2018-01-01

14C is one of the limiting radionuclides used in the categorization of radioactive graphite waste; this categorization is crucial in selecting the appropriate graphite treatment/disposal method. We propose a rapid analysis method for 14C specific activity determination in small graphite samples in the 1-100 μg range. The method applies an oxidation procedure to the sample, which extracts 14C from the different carbonaceous matrices in a controlled manner. Because this method enables fast online measurement and 14C specific activity evaluation, it can be especially useful for characterizing 14C in irradiated graphite when dismantling graphite moderator and reflector parts, or when sorting radioactive graphite waste from decommissioned nuclear power plants. The proposed rapid method is based on graphite combustion and the subsequent measurement of both CO2 and 14C, using a commercial elemental analyser and the semiconductor detector, respectively. The method was verified using the liquid scintillation counting (LSC) technique. The uncertainty of this rapid method is within the acceptable range for radioactive waste characterization purposes. The 14C specific activity determination procedure proposed in this study takes approximately ten minutes, comparing favorably to the more complicated and time consuming LSC method. This method can be potentially used to radiologically characterize radioactive waste or used in biomedical applications when dealing with the specific activity determination of 14C in the sample.

Quality of Graphite Target for Biological/Biomedical/Environmental Applications of 14C-Accelerator Mass Spectrometry

PubMed Central

2010-01-01

Catalytic graphitization for 14C-accelerator mass spectrometry (14C-AMS) produced various forms of elemental carbon. Our high-throughput Zn reduction method (C/Fe = 1:5, 500 °C, 3 h) produced the AMS target of graphite-coated iron powder (GCIP), a mix of nongraphitic carbon and Fe3C. Crystallinity of the AMS targets of GCIP (nongraphitic carbon) was increased to turbostratic carbon by raising the C/Fe ratio from 1:5 to 1:1 and the graphitization temperature from 500 to 585 °C. The AMS target of GCIP containing turbostratic carbon had a large isotopic fractionation and a low AMS ion current. The AMS target of GCIP containing turbostratic carbon also yielded less accurate/precise 14C-AMS measurements because of the lower graphitization yield and lower thermal conductivity that were caused by the higher C/Fe ratio of 1:1. On the other hand, the AMS target of GCIP containing nongraphitic carbon had higher graphitization yield and better thermal conductivity over the AMS target of GCIP containing turbostratic carbon due to optimal surface area provided by the iron powder. Finally, graphitization yield and thermal conductivity were stronger determinants (over graphite crystallinity) for accurate/precise/high-throughput biological, biomedical, and environmental14C-AMS applications such as absorption, distribution, metabolism, elimination (ADME), and physiologically based pharmacokinetics (PBPK) of nutrients, drugs, phytochemicals, and environmental chemicals. PMID:20163100

Chromium Exposure and Hygienic Behaviors in Printing Workers in Southern Thailand

PubMed Central

Decharat, Somsiri

2015-01-01

Objectives. The main objective of this study was to assess the chromium exposure levels in printing workers. The study evaluated the airborne, serum, and urinary chromium levels and determines any correlation between level of chromium in specimen and airborne chromium levels. Material and Methods. A cross-sectional study was conducted with 75 exposed and 75 matched nonexposed subjects. Air breathing zone was measured by furnace atomic absorption spectrophotometer. Serum and urine samples were collected to determine chromium levels by graphite furnaces atomic absorption spectrometer chromium analyzer. Results and Discussion. The printing workers' urinary chromium levels (6.86 ± 1.93 μg/g creatinine) and serum chromium levels (1.24 ± 1.13 μg/L) were significantly higher than the control group (p < 0.001 and p < 0.001). Work position, duration of work, personal protective equipment (PPE), and personal hygiene were significantly associated with urinary chromium level and serum chromium levels (p < 0.001 and p < 0.001). This study found a correlation between airborne chromium levels and urinary chromium levels (r = 0.247, p = 0.032). A multiple regression model was constructed. Significant predictors of urinary and serum chromium levels were shown in this study. Conclusion. Improvements in working conditions, occupational health training, and PPE use are recommended to reduce chromium exposure. PMID:26448746

Principles and practices of irradiation creep experiment using pressurized mini-bellows

DOE Office of Scientific and Technical Information (OSTI.GOV)

Byun, Thak Sang; Li, Meimei; Snead, Lance Lewis

2013-01-01

This article is to describe the key design principles and application practices of the newly developed in-reactor irradiation creep testing technology using pressurized mini-bellows. Miniature creep test frames were designed to fit into the high flux isotope reactor (HFIR) rabbit capsule whose internal diameter is slightly less than 10 mm. The most important consideration for this in-reactor creep testing technology was the ability of the small pressurized metallic bellows to survive irradiation at elevated temperatures while maintaining applied load to the specimen. Conceptual designs have been developed for inducing tension and compression stresses in specimens. Both the theoretical model andmore » the in-furnace test confirmed that a gas-pressurized bellows can produce high enough stress to induce irradiation creep in subsize specimens. Discussion focuses on the possible stress range in specimens induced by the miniature gas-pressurized bellows and the limitations imposed by the size and structure of thin-walled bellows. A brief introduction to the in-reactor creep experiment for graphite is provided to connect to the companion paper describing the application practices and irradiation creep data. An experimental and calculation procedure to obtain in-situ applied stress values from post irradiation in-furnace force measurements is also presented.« less

Study on the early warning mechanism for the security of blast furnace hearths

NASA Astrophysics Data System (ADS)

Zhao, Hong-bo; Huo, Shou-feng; Cheng, Shu-sen

2013-04-01

The campaign life of blast furnace (BF) hearths has become the limiting factor for safety and high efficiency production of modern BFs. However, the early warning mechanism of hearth security has not been clear. In this article, based on heat transfer calculations, heat flux and erosion monitoring, the features of heat flux and erosion were analyzed and compared among different types of hearths. The primary detecting elements, mathematical models, evaluating standards, and warning methods were discussed. A novel early warning mechanism with the three-level quantificational standards was proposed for BF hearth security.

Alkaline electrochemical advanced oxidation process for chromium oxidation at graphitized multi-walled carbon nanotubes.

PubMed

Xue, Yudong; Zheng, Shili; Sun, Zhi; Zhang, Yi; Jin, Wei

2017-09-01

Alkaline electrochemical advanced oxidation processes for chromium oxidation and Cr-contaminated waste disposal were reported in this study. The highly graphitized multi-walled carbon nanotubes g-MWCNTs modified electrode was prepared for the in-situ electrochemical generation of HO 2 - . RRDE test results illustrated that g-MWCNTs exhibited much higher two-electron oxygen reduction activity than other nanocarbon materials with peak current density of 1.24 mA cm -2 , %HO 2 - of 77.0% and onset potential of -0.15 V (vs. Hg/HgO). It was originated from the highly graphitized structure and good electrical conductivity as illustrated from the Raman, XRD and EIS characterizations, respectively. Large amount of reactive oxygen species (HO 2 - and ·OH) were in-situ electro-generated from the two-electron oxygen reduction and chromium-induced alkaline electro-Fenton-like reaction. The oxidation of Cr(III) was efficiently achieved within 90 min and the conversion ratio maintained more than 95% of the original value after stability test, offering an efficient and green approach for the utilization of Cr-containing wastes. Copyright © 2017 Elsevier Ltd. All rights reserved.

Bolt clampup relaxation in a graphite/epoxy laminate

NASA Technical Reports Server (NTRS)

Shivakumar, K. N.; Crews, J. H., Jr.

1982-01-01

A simple bolted joint was analyzed to calculate bolt clampup relaxation for a graphite/epoxy (T300/5208) laminate. A viscoelastic finite element analysis of a double-lap joint with a steel bolt was conducted. Clampup forces were calculated for various steady-state temperature-moisture conditions using a 20-year exposure duration. The finite element analysis predicted that clampup forces relax even for the room-temperature-dry condition. The relaxations were 8, 13, 20, and 30 percent for exposure durations of 1 day, 1 month, 1 year, and 20 years, respectively. As expected, higher temperatures and moisture levels each increased the relaxation rate. The combined viscoelastic effects of steady-state temperature and moisture appeared to be additive. From the finite-element analysis, a simple equation was developed for clampup force relaxation. This generalized equation was used to calculate clampup forces for the same temperature-moisture conditions as used in the finite-element analysis. The two sets of calculated results agreed well.

Searching for magnetism in hydrogenated graphene: using highly hydrogenated graphene prepared via Birch reduction of graphite oxides.

PubMed

Eng, Alex Yong Sheng; Poh, Hwee Ling; Šaněk, Filip; Maryško, Miroslav; Matějková, Stanislava; Sofer, Zdeněk; Pumera, Martin

2013-07-23

Fully hydrogenated graphene (graphane) and partially hydrogenated graphene materials are expected to possess various fundamentally different properties from graphene. We have prepared highly hydrogenated graphene containing 5% wt of hydrogen via Birch reduction of graphite oxide using elemental sodium in liquid NH3 as electron donor and methanol as proton donor in the reduction. We also investigate the influence of preparation method of graphite oxide, such as the Staudenmaier, Hofmann or Hummers methods on the hydrogenation rate. A control experiment involving NaNH2 instead of elemental Na was also performed. The materials were characterized in detail by electron microscopy, infrared spectroscopy, X-ray photoelectron spectroscopy, Raman spectroscopy both at room and low temperatures, X-ray fluorescence spectroscopy, inductively coupled plasma optical emission spectroscopy, combustible elemental analysis and electrical resistivity measurements. Magnetic measurements are provided of bulk quantities of highly hydrogenated graphene. In the whole temperature range up to room temperature, the hydrogenated graphene exhibits a weak ferromagnetism in addition to a contribution proportional to field that is caused not only by diamagnetism but also likely by an antiferromagnetic influence. The origin of the magnetism is also determined to arise from the hydrogenated graphene itself, and not as a result of any metallic impurities.

Development and demonstration of manufacturing processes for fabricating graphite/Larc-160 polyimide structural elements, part 4, paragraph C

NASA Technical Reports Server (NTRS)

1981-01-01

Progress in the development of processes for production of Celion/LARC-160 graphite-polyimide materials, quality control methods, and the fabrication of Space Shuttle composite structure components is reported. The formulation and processing limits for three batches of resin are presented. Process improvements for simplification of the imidizing and autoclave cure cycles are described. Imidized and autoclave cured test panels were prepared. Celion/LARC-160 cure process verification and the fabrication of honeycomb sandwich panel elements and skin/stringer panels are described. C-scans of laminates imidized at 163 C to 218 C for periods from 30 to 180 minutes, and of process verification laminates made from different batches of prepreg are presented. Failure modes and load/strain characteristics of sandwich elements and C-scans of stringer to skin bond joints are also given.

Method of making a modified ceramic-ceramic composite

DOEpatents

Weaver, Billy L.; McLaughlin, Jerry C.; Stinton, David P.

1995-01-01

The present invention provides a method of making a shaped ceramic-ceramic composite articles, such as gas-fired radiant heat burner tubes, heat exchangers, flame dispersers, and other furnace elements, having a formed-on ceramic-ceramic composite thereon.

Extraterrestrial processing and manufacturing of large space systems, volume 2, chapters 7-14 and appendices

NASA Technical Reports Server (NTRS)

Miller, R. H.; Smith, D. B. S.

1979-01-01

Production and support equipment specifications are described for the space manufacturing facility (SMF). Defined production equipment includes electromagnetic pumps for liquid metal, metal alloying furnaces, die casters, electron beam welders and cutters, glass forming for structural elements, and rolling. A cost analysis is presented which includes the development, the aquisition of all SMF elements, initial operating cost, maintenance and logistics cost, cost of terrestrial materials, and transportation cost for each major element. Computer program listings and outputs are appended.

Preparation of thin film silver fluoride electrodes from constituent elements

NASA Technical Reports Server (NTRS)

Odonnell, P. M.

1972-01-01

The feasibility of preparing thin-film metal fluoride electrodes from the elemental constituents has been demonstrated. Silver fluoride cathodes were prepared by deposition of silver on a conducting graphite substrate followed by fluorination under controlled conditions using elemental fluorine. The resulting electrodes were of high purity, and the variables such as size, shape, and thickness were easily controlled.

Growth rates and interface shapes in germanium and lead tin telluride observed in-situ, real-time in vertical Bridgman furnaces

NASA Technical Reports Server (NTRS)

Barber, P. G.; Berry, R. F.; Debnam, W. J.; Fripp, A. L.; Woodell, G.; Simchick, R. T.

1995-01-01

Using the advanced technology developed to visualize the melt-solid interface in low Prandtl number materials, crystal growth rates and interface shapes have been measured in germanium and lead tin telluride semiconductors grown in vertical Bridgman furnaces. The experimental importance of using in-situ, real time observations to determine interface shapes, to measure crystal growth rates, and to improve furnace and ampoule designs is demonstrated. The interface shapes observed in-situ, in real-time were verified by quenching and mechanically induced interface demarcation, and they were also confirmed using machined models to ascertain the absence of geometric distortions. Interface shapes depended upon the interface position in the furnace insulation zone, varied with the nature of the crystal being grown, and were dependent on the extent of transition zones at the ends of the ampoule. Actual growth rates varied significantly from the constant translation rate in response to the thermophysical properties of the crystal and its melt and the thermal conditions existing in the furnace at the interface. In the elemental semiconductor germanium the observed rates of crystal growth exceeded the imposed translation rate, but in the compound semiconductor lead tin telluride the observed rates of growth were less than the translation rate. Finally, the extent of ampoule thermal loading influenced the interface positions, the shapes, and the growth rates.

Ancient graphite in the Eoarchean quartz-pyroxene rocks from Akilia in southern West Greenland II: Isotopic and chemical compositions and comparison with Paleoproterozoic banded iron formations

NASA Astrophysics Data System (ADS)

Papineau, Dominic; De Gregorio, Bradley T.; Stroud, Rhonda M.; Steele, Andrew; Pecoits, Ernesto; Konhauser, Kurt; Wang, Jianhua; Fogel, Marilyn L.

2010-10-01

We present detailed petrographic surveys of apatite grains in association with carbonaceous material (CM) in two banded iron formations (BIFs) from the Paleoproterozoic of Uruguay and Michigan for comparison with similar mineral associations in the highly debated Akilia Quartz-pyroxene (Qp) rock. Petrographic and Raman spectroscopic surveys of these Paleoproterozoic BIFs show that apatite grains typically occur in bands parallel to bedding and are more often associated with CM when concentrations of organic matter are high. Carbonaceous material in the Vichadero BIF from Uruguay is generally well-crystallized graphite and occurs in concentrations around 0.01 wt% with an average δ 13C gra value of -28.6 ± 4.4‰ (1 σ). In this BIF, only about 5% of apatite grains are associated with graphite. In comparison, CM in the Bijiki BIF from Michigan is also graphitic, but occurs in concentrations around 2.4 wt% with δ 13C gra values around -24.0 ± 0.3‰ (1 σ). In the Bijiki BIF, more than 78% of apatite grains are associated with CM. Given the geologic context and high levels of CM in the Bijiki BIF, the significantly higher proportion of apatite grains associated with CM in this rock is interpreted to represent diagenetically altered biomass and shows that such diagenetic mineral associations can survive metamorphism up to the amphibolite facies. Isotope compositions of CM in muffled acidified whole-rock powders from the Akilia Qp rock have average δ 13C gra values of -17.5 ± 2.5‰ (1 σ), while δ 13C carb values in whole-rock powders average -4.0 ± 1.0‰ (1 σ). Carbon isotope compositions of graphite associated with apatite and other minerals in the Akilia Qp rock were also measured with the NanoSIMS to have similar ranges of δ 13C gra values averaging -13.8 ± 5.6‰ (1 σ). The NanoSIMS was also used to semi-quantitatively map the distributions of H, N, O, P, and S in graphite from the Akilia Qp rock, and relative abundances were found to be similar for graphite associated with apatite or with hornblende, calcite, and sulfides. These analyses revealed generally lower abundances of trace elements in the Akilia graphite compared to graphite associated with apatite from Paleoproterozoic BIFs. Graphite associated with hornblende, calcite, and sulfides in the Akilia Qp rock was fluid-deposited at high-temperature from carbon-bearing fluids, and since this graphite has similar ranges of δ 13C gra values and of trace elements compared to graphite associated with apatite, we conclude that the Akilia graphite in different mineral associations formed from the same source(s) of CM. Collectively our results do not exclude a biogenic origin of the carbon in the Akilia graphite, but because some observations can not exclude graphitization of abiogenic carbon from CO 2- and CH 4-bearing mantle fluids, there remain ambiguities with respect to the exact origin of carbon in this ancient metasedimentary rock. Accordingly, there may have been several generations of graphite formation along with possibly varying mixtures of CO 2- and CH 4-bearing fluids that may have resulted in large ranges of δ 13C gra values. The possibility of fluid-deposited graphite associated with apatite should be a focus of future investigations as this may prove to be an alternative pathway of graphitization from phosphate-bearing fluids. Correlated micro-analytical approaches tested on terrestrial rocks in this work provide insights into the origin of carbon in ancient graphite and will pave the way for the search for life on other ancient planetary surfaces.

Empirical potential for molecular simulation of graphene nanoplatelets

NASA Astrophysics Data System (ADS)

Bourque, Alexander J.; Rutledge, Gregory C.

2018-04-01

A new empirical potential for layered graphitic materials is reported. Interatomic interactions within a single graphene sheet are modeled using a Stillinger-Weber potential. Interatomic interactions between atoms in different sheets of graphene in the nanoplatelet are modeled using a Lennard-Jones interaction potential. The potential is validated by comparing molecular dynamics simulations of tensile deformation with the reported elastic constants for graphite. The graphite is found to fracture into graphene nanoplatelets when subjected to ˜15% tensile strain normal to the basal surface of the graphene stack, with an ultimate stress of 2.0 GPa and toughness of 0.33 GPa. This force field is useful to model molecular interactions in an important class of composite systems comprising 2D materials like graphene and multi-layer graphene nanoplatelets.

Adaptive control of interface by temperature and interface profile feedback in transparent multi-zone crystal growth furnace

NASA Technical Reports Server (NTRS)

Batur, Celal

1991-01-01

The objective of this research is to control the dynamics of multizone programmable crystal growth furnaces. Due to the inevitable heat exchange among different heating zones and the transient nature of the process, the dynamics of multizone furnaces is time varying, distributed, and therefore complex in nature. Electrical power to heating zones and the translational speed of the ampoule are employed as inputs to control the dynamics. Structural properties of the crystal is the ultimate aim of this adaptive control system. These properties can be monitored in different ways. Following an order of complexity, these may include: (1) on line measurement of the material optical properties such as the refractive index of crystal; (2) on line x-ray imaging of the interface topology; (3) on line optical quantification of the interface profile such as the determination of concavity or convexity of the interface shape; and (4) on line temperature measurement at points closest to the material such as measurements of the ampoule's outside and inside surface temperatures. The research performed makes use of the temperature and optical measurements, specified in (3) and (4) as the outputs of furnace dynamics. However, if the instrumentation is available, the proposed control methodology can be extended to the measurements listed in (1) and (2).

Material property for designing, analyzing, and fabricating space structures

NASA Technical Reports Server (NTRS)

Kolkailah, Faysal A.

1991-01-01

An analytical study was made of plasma assisted bullet projectile. The finite element analysis and the micro-macromechanic analysis was applied to an optimum design technique for the multilayered graphite-epoxy composite projectile that will achieve hypervelocity of 6 to 10 Km/s. The feasibility was determined of dialectics to monitor cure of graphite-epoxies. Several panels were fabricated, cured, and tested with encouraging results of monitoring the cure of graphite-epoxies. The optimum cure process for large structures was determined. Different orientation were used and three different curing cycles were employed. A uniaxial tensile test was performed on all specimens. The optimum orientation with the optimum cure cycle were concluded.

[Determination of lead in edible salt with solid-phase extraction and GFAAS].

PubMed

Zhao, Xin; Zhou, Shuang; Ma, Lan; Yang, Dajin

2013-01-01

Establishing a method for determination of lead in salt with solid-phase extraction and GFAAS. Salt sample was diluted to a certain volume directly with ammonium acetate, then the sample solution was filtered through the solid phase extraction column which has been pre-activated. Lead ions were retained, and the sodium chloride matrix was removed. After elution, the collected lead ions was determined by graphite furnace atomic absorption spectrometry in 257.4 nm. This method can be used effectively to wipe off the sodium chloride in matrix. The limit of detection was 0.7 microg/kg and the limit of quantification was 2 microg/kg. Solid phase extraction technique can be used effectively to reduce the interference in matrix and improves the accuracy and reproducibility of detection.

[Development of ICP-OES, ICP-MS and GF-AAS Methods for Simultaneous Quantification of Lead, Total Arsenic and Cadmium in Soft Drinks].

PubMed

Kataoka, Yohei; Watanabe, Takahiro; Hayashi, Tomoko; Teshima, Reiko; Matsuda, Rieko

2015-01-01

In this study, we developed methods to quantify lead, total arsenic and cadmium contained in various kinds of soft drinks, and we evaluated their performance. The samples were digested by common methods to prepare solutions for measurement by ICP-OES, ICP-MS and graphite furnace atomic absorption spectrometry (GF-AAS). After digestion, internal standard was added to the digestion solutions for measurements by ICP-OES and ICP-MS. For measurement by GF-AAS, additional purification of the digestion solution was conducted by back-extraction of the three metals into nitric acid solution after extraction into an organic solvent with ammonium pyrrolidine dithiocarbamate. Performance of the developed methods were evaluated for eight kinds of soft drinks.

Sulfur-doped graphene via thermal exfoliation of graphite oxide in H2S, SO2, or CS2 gas.

PubMed

Poh, Hwee Ling; Šimek, Petr; Sofer, Zdeněk; Pumera, Martin

2013-06-25

Doping of graphene with heteroatoms is an effective way to tailor its properties. Here we describe a simple and scalable method of doping graphene lattice with sulfur atoms during the thermal exfoliation process of graphite oxides. The graphite oxides were first prepared by Staudenmaier, Hofmann, and Hummers methods followed by treatments in hydrogen sulfide, sulfur dioxide, or carbon disulfide. The doped materials were characterized by scanning electron microscopy, high-resolution X-ray photoelectron spectroscopy, combustible elemental analysis, and Raman spectroscopy. The ζ-potential and conductivity of sulfur-doped graphenes were also investigated in this paper. It was found that the level of doping is more dramatically influenced by the type of graphite oxide used rather than the type of sulfur-containing gas used during exfoliation. Resulting sulfur-doped graphenes act as metal-free electrocatalysts for an oxygen reduction reaction.

High temperature gradient cobalt based clad developed using microwave hybrid heating

NASA Astrophysics Data System (ADS)

Prasad, C. Durga; Joladarashi, Sharnappa; Ramesh, M. R.; Sarkar, Anunoy

2018-04-01

The development of cobalt based cladding on a titanium substrate using microwave cladding technique is benchmark in coating area. The developed cladding would serve the function of a corrosion resistant coating under high temperatures. Clads of thickness 500 µm have been developed by microwave hybrid heating. A microwave furnace of 2.45GHz frequency was used at a 900W power level for processing. Impact of processing time on melting and adhesion of clad has been discussed. The study also extended to static thermal analysis of simple parts with cladding using commercial Finite Element analysis (FEA) software. A comparative study is explored between four variants of the clad being developed. The analysis has been conducted using a square sample. Similar temperature gradient is also shown for a proposed multi-layer coating, which includes a thermal barrier coating yttria stabilized zirconia (YSZ) on top of the corrosion resistant clad. The YSZ coating would protect the corrosion resistant cladding and substrate from high temperatures.

An innovative method for nondestructive analysis of cast iron artifacts at Hopewell Furnace National Historic Site, Pennsylvania

USGS Publications Warehouse

Sloto, R.A.; Helmke, M.F.

2011-01-01

Iron ore containing elevated concentrations of trace metals was smelted at Hopewell Furnace during its 113 years of operation (1771-1883). For this study, we sampled iron ore, cast iron furnace products, slag, soil, groundwater, streamflow, and streambed sediment to determine the fate of trace metals released into the environment during the iron-smelting process. Standard techniques were used to sample and analyze all media except cast iron. We analyzed the trace-metal content of the cast iron using a portable X-ray fluorescence spectrometer, which provided rapid, on-site, nondestructive analyses for 23 elements. The artifacts analyzed included eight cast iron stoves, a footed pot, and a kettle in the Hopewell Furnace museum. We measured elevated concentrations of arsenic, copper, lead, and zinc in the cast iron. Lead concentrations as great as 3,150 parts per million were measured in the stoves. Cobalt was detectable but not quantifiable because of interference with iron. Our study found that arsenic, cobalt, and lead were not released to soil or slag, which could pose a significant health risk to visitors and employees. Instead, our study demonstrates these heavy metals remained with the cast iron and were removed from the site.

Removal of Oxygen from Electronic Materials by Vapor-Phase Processes

NASA Technical Reports Server (NTRS)

Palosz, Witold

1997-01-01

Thermochemical analyses of equilibrium partial pressures over oxides with and without the presence of the respective element condensed phase, and hydrogen, chalcogens, hydrogen chalcogenides, and graphite are presented. Theoretical calculations are supplemented with experimental results on the rate of decomposition and/or sublimation/vaporization of the oxides under dynamic vacuum, and on the rate of reaction with hydrogen, graphite, and chalcogens. Procedures of removal of a number of oxides under different conditions are discussed.

Electron paramagnetic resonance field-modulation eddy-current analysis of silver-plated graphite resonators

NASA Astrophysics Data System (ADS)

Mett, Richard R.; Anderson, James R.; Sidabras, Jason W.; Hyde, James S.

2005-09-01

Magnetic field modulation is often introduced into a cylindrical TE011 electron paramagnetic resonance (EPR) cavity through silver plating over a nonconductive substrate. The plating thickness must be many times the skin depth of the rf and smaller than the skin depth of the modulation. We derive a parameter that quantifies the modulation field penetration and find that it also depends on resonator dimensions. Design criteria based on this parameter are presented graphically. This parameter is then used to predict the behavior of eddy currents in substrates of moderate conductivity, such as graphite. The conductivity of the graphite permits improved plating uniformity and permits use of electric discharge machining (EDM) techniques to make the resonator. EDM offers precision tolerances of 0.005 mm and is suitable for small, complicated shapes that are difficult to machine by other methods. Analytic predictions of the modulation penetration are compared with the results of finite-element simulations. Simulated magnetic field modulation uniformity and penetration are shown for several elemental coils and structures including the plated graphite TE011 cavity. Fabrication and experimental testing of the structure are discussed. Spatial inhomogeneity of the modulation phase is also investigated by computer simulation. We find that the modulation phase is uniform to within 1% over the TE011 cavity. Structures of lower symmetry have increased phase nonuniformity.

Trace elements and metals in farmed sea bass and gilthead bream from Tenerife Island, Spain.

PubMed

Rubio, C; Jalilli, A; Gutiérrez, A J; González-Weller, D; Hernández, F; Melón, E; Burgos, A; Revert, C; Hardisson, A

2011-11-01

The aim of this study was to determine the levels of metals (Ca, K, Na, Mg) and trace metals (Ni, Fe, Cu, Mn, Zn, Pb, Cd) in two fish species (gilthead bream [Sparus aurata] and sea bass [Dicentrarchus labrax]) collected from fish farms located along the coast of Tenerife Island. Ca, K, Na, Mg, Fe, Cu, Zn, and Mn were measured by flame atomic absorption spectrometry, whereas Pb, Cd, and Ni were determined using graphite furnace atomic absorption spectrometry. Mean Fe, Cu, Mn, and Zn contents were 3.09, 0.59, 0.18, and 8.11 mg/kg (wet weight) in S. aurata and 3.20, 0.76, 0.24, and 10.11 mg/kg (wet weight) in D. labrax, respectively. In D. labrax, Ca, K, Na, and Mg levels were 1,955, 2,787, 699.7, and 279.2 mg/kg (wet weight), respectively; in S. aurata, they were 934.7, 3,515, 532.8, and 262.8 mg/kg (wet weight), respectively. The Pb level in S. aurata was 7.28 ± 3.64 μg/kg (wet weight) and, in D. labrax, 4.42 ± 1.56 μg/kg (wet weight). Mean Cd concentrations were 3.33 ± 3.93 and 1.36 ± 1.53 μg/kg (wet weight) for D. labrax and S. aurata, respectively. All Pb and Cd levels measured were well below the accepted European Commission limits, 300 and 50 μg/kg for lead and cadmium, respectively.

Identifying the origins of local atmospheric deposition in the steel industry basin of Luxembourg using the chemical and isotopic composition of the lichen Xanthoria parietina.

PubMed

Hissler, Christophe; Stille, Peter; Krein, Andreas; Geagea, Majdi Lahd; Perrone, Thierry; Probst, Jean-Luc; Hoffmann, Lucien

2008-11-01

Trace metal atmospheric contamination was assessed in one of the oldest European industrial sites of steel production situated in the southern part of the Grand-Duchy of Luxembourg. Using elemental ratios as well as Pb, Sr, and Nd isotopic compositions as tracers, we found preliminary results concerning the trace metal enrichment and the chemical/isotopic signatures of the most important emission sources using the lichen Xanthoria parietina sampled at 15 sites along a SW-NE transect. The concentrations of these elements decreased with increasing distance from the historical and actual steel-work areas. The combination of the different tracers (major elements, Rare Earth Element ratios, Pb, Sr and Nd isotopes) enabled us to distinguish between three principal sources: the historical steel production (old tailings corresponding to blast-furnace residues), the present steel production (industrial sites with arc electric furnace units) and the regional background (baseline) components. Other anthropogenic sources including a waste incinerator and major roads had only weak impacts on lichen chemistry and isotopic ratios. The correlation between the Sr and Nd isotope ratios indicated that the Sr-Nd isotope systems represented useful tools to trace atmospheric emissions of factories using scrap metal for steel production.

Understanding the Growth Mechanism of GaN Epitaxial Layers on Mechanically Exfoliated Graphite

NASA Astrophysics Data System (ADS)

Li, Tianbao; Liu, Chenyang; Zhang, Zhe; Yu, Bin; Dong, Hailiang; Jia, Wei; Jia, Zhigang; Yu, Chunyan; Gan, Lin; Xu, Bingshe; Jiang, Haiwei

2018-04-01

The growth mechanism of GaN epitaxial layers on mechanically exfoliated graphite is explained in detail based on classic nucleation theory. The number of defects on the graphite surface can be increased via O-plasma treatment, leading to increased nucleation density on the graphite surface. The addition of elemental Al can effectively improve the nucleation rate, which can promote the formation of dense nucleation layers and the lateral growth of GaN epitaxial layers. The surface morphologies of the nucleation layers, annealed layers and epitaxial layers were characterized by field-emission scanning electron microscopy, where the evolution of the surface morphology coincided with a 3D-to-2D growth mechanism. High-resolution transmission electron microscopy was used to characterize the microstructure of GaN. Fast Fourier transform diffraction patterns showed that cubic phase (zinc-blend structure) GaN grains were obtained using conventional GaN nucleation layers, while the hexagonal phase (wurtzite structure) GaN films were formed using AlGaN nucleation layers. Our work opens new avenues for using highly oriented pyrolytic graphite as a substrate to fabricate transferable optoelectronic devices.

Understanding the Growth Mechanism of GaN Epitaxial Layers on Mechanically Exfoliated Graphite.

PubMed

Li, Tianbao; Liu, Chenyang; Zhang, Zhe; Yu, Bin; Dong, Hailiang; Jia, Wei; Jia, Zhigang; Yu, Chunyan; Gan, Lin; Xu, Bingshe; Jiang, Haiwei

2018-04-27

The growth mechanism of GaN epitaxial layers on mechanically exfoliated graphite is explained in detail based on classic nucleation theory. The number of defects on the graphite surface can be increased via O-plasma treatment, leading to increased nucleation density on the graphite surface. The addition of elemental Al can effectively improve the nucleation rate, which can promote the formation of dense nucleation layers and the lateral growth of GaN epitaxial layers. The surface morphologies of the nucleation layers, annealed layers and epitaxial layers were characterized by field-emission scanning electron microscopy, where the evolution of the surface morphology coincided with a 3D-to-2D growth mechanism. High-resolution transmission electron microscopy was used to characterize the microstructure of GaN. Fast Fourier transform diffraction patterns showed that cubic phase (zinc-blend structure) GaN grains were obtained using conventional GaN nucleation layers, while the hexagonal phase (wurtzite structure) GaN films were formed using AlGaN nucleation layers. Our work opens new avenues for using highly oriented pyrolytic graphite as a substrate to fabricate transferable optoelectronic devices.

Extraction of mineral elements from inedible wastes of biological components of a life-support system and their utilization for plant nutrition

NASA Astrophysics Data System (ADS)

Gribovskaya, I. V.; Gladchenko, I. A.; Zinenko, G. K.

Two methods of extracting mineral elements from otherwise deadlock products of a life-support system are presented. We describe first optimum conditions for recovering elements by water extraction from dry wastes of plants, biomass ash, and solid human wastes after passing them through the catalytic furnace; and, second, we describe acid extracts of biogenous elements by 1N and 2N HNO_3 from these products. Ways to use the extracts of elements in plant nutrition are considered in order to increase the extent to which the mineral loop of a life-support system can be closed.

Finite Element Creep-Fatigue Analysis of a Welded Furnace Roll for Identifying Failure Root Cause

NASA Astrophysics Data System (ADS)

Yang, Y. P.; Mohr, W. C.

2015-11-01

Creep-fatigue induced failures are often observed in engineering components operating under high temperature and cyclic loading. Understanding the creep-fatigue damage process and identifying failure root cause are very important for preventing such failures and improving the lifetime of engineering components. Finite element analyses including a heat transfer analysis and a creep-fatigue analysis were conducted to model the cyclic thermal and mechanical process of a furnace roll in a continuous hot-dip coating line. Typically, the roll has a short life, <1 year, which has been a problem for a long time. The failure occurred in the weld joining an end bell to a roll shell and resulted in the complete 360° separation of the end bell from the roll shell. The heat transfer analysis was conducted to predict the temperature history of the roll by modeling heat convection from hot air inside the furnace. The creep-fatigue analysis was performed by inputting the predicted temperature history and applying mechanical loads. The analysis results showed that the failure was resulted from a creep-fatigue mechanism rather than a creep mechanism. The difference of material properties between the filler metal and the base metal is the root cause for the roll failure, which induces higher creep strain and stress in the interface between the weld and the HAZ.

The aluminium content of breast tissue taken from women with breast cancer.

PubMed

House, Emily; Polwart, Anthony; Darbre, Philippa; Barr, Lester; Metaxas, George; Exley, Christopher

2013-10-01

The aetiology of breast cancer is multifactorial. While there are known genetic predispositions to the disease it is probable that environmental factors are also involved. Recent research has demonstrated a regionally specific distribution of aluminium in breast tissue mastectomies while other work has suggested mechanisms whereby breast tissue aluminium might contribute towards the aetiology of breast cancer. We have looked to develop microwave digestion combined with a new form of graphite furnace atomic absorption spectrometry as a precise, accurate and reproducible method for the measurement of aluminium in breast tissue biopsies. We have used this method to test the thesis that there is a regional distribution of aluminium across the breast in women with breast cancer. Microwave digestion of whole breast tissue samples resulted in clear homogenous digests perfectly suitable for the determination of aluminium by graphite furnace atomic absorption spectrometry. The instrument detection limit for the method was 0.48 μg/L. Method blanks were used to estimate background levels of contamination of 14.80 μg/L. The mean concentration of aluminium across all tissues was 0.39 μg Al/g tissue dry wt. There were no statistically significant regionally specific differences in the content of aluminium. We have developed a robust method for the precise and accurate measurement of aluminium in human breast tissue. There are very few such data currently available in the scientific literature and they will add substantially to our understanding of any putative role of aluminium in breast cancer. While we did not observe any statistically significant differences in aluminium content across the breast it has to be emphasised that herein we measured whole breast tissue and not defatted tissue where such a distribution was previously noted. We are very confident that the method developed herein could now be used to provide accurate and reproducible data on the aluminium content in defatted tissue and oil from such tissues and thereby contribute towards our knowledge on aluminium and any role in breast cancer. Copyright © 2013 Elsevier GmbH. All rights reserved.

[Determination of lead in microemulsified rapeseed oil and bio-diesel oil by GFAAS].

PubMed

Li, Sheng-qing; He, Xiao-min; Du, Ping; Wang, Min; Chen, Hao; Wu, Mou-cheng

2008-10-01

Bio-diesel oil has attracted much attention as a substitutable energy sources for its renewable and eco-friendly property. However, problems of lead contamination in fuel are also emphasized increasingly at present. So it was of quite significance to determine the contents of lead in bio-diesel oil and its raw material rapeseed oil. An effective method was developed for the rapid determination of lead in rapeseed oil and bio-diesel oil by graphite furnace atomic absorption spectrometry (GFAAS) after their stabilization as microemulsions. In this research work, polyethyleneglycol octyl phenyl ether and n-butanol were used for emulsifier and auxiliary emulsifying agent, respectively. For Pb, efficient thermal stabilization was obtained using NH4H2PO4 as matrix modifier. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization and the influence of the microemulsion composition on the GFAAS response were observed by mixing different organic solvents. The ashing and atomization temperature and ramp rate influenced the sensitivity obtained for Ph. Take this into account, the optimum conditions of the graphite furnace atomic absorption spectrometric determination of Pb in rapeseed oil and bio-diesel oil samples were investigated. The results showed that the microemulsion was quite stable when the value of V(20% polyethyleneglycol octyl phenyl ether), V(n-butanol), V(oil) and V(water) was 0.1: 8.9: 0.5: 0.5, without matrix interference effect. The determination limit of the proposed method was 126.2 microg x L(-1) for Pb, comfortably below the values found in the analyzed samples. The recoveries were from 81.8% to 109.0%, which performed using the addition of different concentrations of lead to bio-diesel oil, rapeseed oil and petrochemical diesel samples. The relative standard deviation of determination was 5.84%. This work showed the great efficiency of the microemulsion, indicating that it is possible to extract lead from the oil phase. The method was applied to the determination of lead in oil samples with satisfactory results.

Single-Step, Solvent-Free, Catalyst-Free Preparation of Holey Carbon Allotropes

NASA Technical Reports Server (NTRS)

Lin, Yi (Inventor); Funk, Michael R. (Inventor); Kim, Jae-Woo (Inventor); Connell, John W. (Inventor); Campbell, Caroline J. (Inventor)

2017-01-01

Methods for forming holey carbon allotropes and graphene nanomeshes are provided by the various embodiments. The various embodiments may be applicable to a variety of carbon allotropes, such as graphene, graphene oxide, reduced graphene oxide, thermal exfoliated graphene, graphene nanoribbons, graphite, exfoliated graphite, expanded graphite, carbon nanotubes (e.g., single-walled carbon nanotubes, double-walled carbon nanotubes, few-walled carbon nanotubes, multi-walled carbon nanotubes, etc.), carbon nanofibers, carbon fibers, carbon black, amorphous carbon, fullerenes, etc. The methods may produce holey carbon allotropes without the use of solvents, catalysts, flammable gas, additional chemical agents, or electrolysis to produce the pores (e.g., holes, etc.) in the carbon allotropes. In an embodiment, a carbon allotrope may be heated at a working window temperature for a working period of time to create holes in the carbon allotrope.

Carbon-oxygen reaction efficiency in air gap switch with graphite electrodes under high current pulse discharge

NASA Astrophysics Data System (ADS)

Dai, Hongyu; Li, Lee; Peng, Ming-yang; Xiong, Jiaming; Wu, Haibo; Yu, Bin

2017-12-01

In order to reduce the effect of residual carbon on the insulation performance, after the GW-hundreds kiloampere graphite-electrode switch turning on, the chemical kinetics of the carbon-oxygen reaction is analyzed. The capacitive pulsed experimental circuit is used to reconstruct the actual condition of high power and high current discharge. The carbon-oxygen reaction efficiency is analyzed using a Fourier transform infrared spectrometer and a flue gas analyzer. The research shows that the gas products include NOX, O3, CH4, and COX. Through the quantitative analysis, the conversion efficiency of COX increases with the augment of the accumulated transferred charge, and the change law of the CO generation efficiency has an extreme value. With the corresponding calculation and the observation of the scanning electron microscope, it is found that most of the carbon consumed from the graphite electrodes is converted to amorphous elemental carbon, and the insufficiency of the carbon-oxygen reaction leads to the problem of carbon residue, for 20%-45% of elemental carbon is not oxidized. The size of amorphous elemental carbon is about several micrometers to tens micrometers by the analysis of metallographic microscope. In the condition of compressed air, changing the amount of transferred charge is helpful to improve the carbon-oxygen reaction efficiency and inhibit the problem of carbon residue.

Origin of the eclogitic clasts with graphite-bearing and graphite-free lithologies in the Northwest Africa 801 (CR2) chondrite: Possible origin from a Moon-sized planetary body inferred from chemistry, oxygen isotopes and REE abundances

NASA Astrophysics Data System (ADS)

Hiyagon, H.; Sugiura, N.; Kita, N. T.; Kimura, M.; Morishita, Y.; Takehana, Y.

2016-08-01

In order to clarify the origin of the eclogitic clasts found in the NWA801 (CR2) chondrite (Kimura et al., 2013), especially, that of the high pressure and temperature (P-T) condition (∼3 GPa and ∼1000 °C), we conducted ion microprobe analyses of oxygen isotopes and rare earth element (REE) abundances in the clasts. Oxygen isotopic compositions of the graphite-bearing lithology (GBL) and graphite-free lithology (GFL) show a slope ∼0.6 correlation slightly below the CR-CH-CB chondrites field in the O three-isotope-diagram, with a large variation for the former and almost homogeneous composition for the latter. The average REE abundances of the two lithologies show almost unfractionated patterns. Based on these newly obtained data, as well as mineralogical observations, bulk chemistry, and considerations about diffusion timescales for various elements, we discuss in detail the formation history of the clasts. Consistency of the geothermobarometers used by Kimura et al. (2013), suggesting equilibration of various elements among different mineral pairs, provides a strong constraint for the duration of the high P-T condition. We suggest that the high P-T condition lasted 102-103 years. This clearly precludes a shock high pressure (HP) model, and hence, strongly supports a static HP model. A static HP model requires a Moon-sized planetary body of ∼1500 km in radius. Furthermore, it implies two successive violent collisions, first at the formation of the large planetary body, when the clasts were placed its deep interior, and second, at the disruption of the large planetary body, when the clasts were expelled out of the parent body and later on transported to the accretion region of the CR chondrites. We also discuss possible origin of O isotopic variations in GBL, and presence/absence of graphite in GBL/GFL, respectively, in relation to smelting possibly occurred during the igneous process(es) which formed the two lithologies. Finally we present a possible formation scenario of the eclogitic clasts.

Carbon Isotopic Heterogeneity of Graphite in the San Juan Mass of the Campo Del Cielo IAB Iron Meteorite

NASA Technical Reports Server (NTRS)

Maruoka, T.; Kurat, G.; Zinner, E.; Varela, M. E.; Ametrano, S. J.

2003-01-01

The origin of IAB iron meteorites is still a matter of debate. It is generally believed that iron meteorites originated from molten cores in small planetesimals because the fractionation trend of trace elements (e.g., Ir, Ge, Ga, etc. vs. Ni) for most iron meteorites can be more or less explained by fractional crystallization from metal melts. However, this process cannot produce trace element characteristics of the IAB (and other) iron meteorites. To explain these trace element abundance patterns, several models have been proposed. Although most of these models require a high temperature, clear evidence has recently been obtained for a sub-solidus formation of IAB iron meteorites from noble gas analyses. Moreover, heterogeneous distributions of some trace elements in metal and other phases also suggest a low temperature origin of at least some IAB iron meteorites. Here we use the carbon isotopic compositions of graphite to constrain the origin of IAB iron meteorites. Our data confirm a possible low temperature origin of IAB iron meteorites.

Design Study of a Modular Gas-Cooled, Closed-Brayton Cycle Reactor for Marine Use

DTIC Science & Technology

1989-06-01

materials in the core and surroundings. To investigate this design point in the marine variant I developed the program HEAT.BAS to perform a one-dimensional...helium as the working fluid. The core is a graphite moderated, epithermal spectrum reactor, using TRISO fuel particles in extruded graphite fuel elements...The fuel is highly enriched U2315 . The containment is shaped in an inverted ’T’ with two sections. The upper section contains the reactor core