Fluorometric determination of zirconium in minerals

Science.gov (United States)

Alford, W.C.; Shapiro, L.; White, C.E.

1951-01-01

The increasing use of zirconium in alloys and in the ceramics industry has created renewed interest in methods for its determination. It is a common constituent of many minerals, but is usually present in very small amounts. Published methods tend to be tedious, time-consuming, and uncertain as to accuracy. A new fluorometric procedure, which overcomes these objections to a large extent, is based on the blue fluorescence given by zirconium and flavonol in sulfuric acid solution. Hafnium is the only element that interferes. The sample is fused with borax glass and sodium carbonate and extracted with water. The residue is dissolved in sulfuric acid, made alkaline with sodium hydroxide to separate aluminum, and filtered. The precipitate is dissolved in sulfuric acid and electrolysed in a Melaven cell to remove iron. Flavonol is then added and the fluorescence intensity is measured with a photo-fluorometer. Analysis of seven standard mineral samples shows excellent results. The method is especially useful for minerals containing less than 0.25% zirconium oxide.

Preparation and application of zirconium sulfate supported on SAPO-34 molecular sieve as solid acid catalyst for esterification

Energy Technology Data Exchange (ETDEWEB)

Xu, Dongyan, E-mail: xdy0156@sina.com; Ma, Hong; Cheng, Fei

2014-05-01

Graphical abstract: - Highlights: • SAPO-34 supported zirconium sulfate solid acid catalyst was prepared. • Esterification of acetic acid with ethanol can be catalyzed by ZS/SAPO-34. • The hydration of ZS is vital to the acidic property and catalytic performance. • The ZS/SAPO-34 catalyst treated at 200 °C shows good reusability. - Abstract: Zirconium sulfate (ZS) was supported on SAPO-34 molecular sieve by using an incipient wetness impregnation method with zirconium sulfate as the precursor. The as-prepared catalysts were used as solid acid catalyst for esterification reaction of acetic acid with ethanol. The influence of calcination temperature on the acidic property, catalytic activity, and reusability of ZS/SAPO-34 catalysts were mainly investigated. FT-IR, SEM, EDS and TG analysis have been carried out to demonstrate the characteristics of ZS/SAPO-34 catalysts. It was found that the 30 wt%ZS/SAPO-34 catalysts display the property of superacid irrespective of calcination temperature. The ZS/SAPO-34 catalyst treated at 200 °C can enhance the interaction between the supported ZS and SAPO-34 and keep the catalyst remaining substantially active after several reaction cycles. However, further increasing calcination temperature will cause the transfer of ZS from hydrate to anhydrous phase, and thus the decrease of activity.

Preparation and application of zirconium sulfate supported on SAPO-34 molecular sieve as solid acid catalyst for esterification

International Nuclear Information System (INIS)

Xu, Dongyan; Ma, Hong; Cheng, Fei

2014-01-01

Graphical abstract: - Highlights: • SAPO-34 supported zirconium sulfate solid acid catalyst was prepared. • Esterification of acetic acid with ethanol can be catalyzed by ZS/SAPO-34. • The hydration of ZS is vital to the acidic property and catalytic performance. • The ZS/SAPO-34 catalyst treated at 200 °C shows good reusability. - Abstract: Zirconium sulfate (ZS) was supported on SAPO-34 molecular sieve by using an incipient wetness impregnation method with zirconium sulfate as the precursor. The as-prepared catalysts were used as solid acid catalyst for esterification reaction of acetic acid with ethanol. The influence of calcination temperature on the acidic property, catalytic activity, and reusability of ZS/SAPO-34 catalysts were mainly investigated. FT-IR, SEM, EDS and TG analysis have been carried out to demonstrate the characteristics of ZS/SAPO-34 catalysts. It was found that the 30 wt%ZS/SAPO-34 catalysts display the property of superacid irrespective of calcination temperature. The ZS/SAPO-34 catalyst treated at 200 °C can enhance the interaction between the supported ZS and SAPO-34 and keep the catalyst remaining substantially active after several reaction cycles. However, further increasing calcination temperature will cause the transfer of ZS from hydrate to anhydrous phase, and thus the decrease of activity

Experimental studies of relevance on zirconium nitrate raffinate sludge for its disposal as well as zirconium recovery

International Nuclear Information System (INIS)

Brahmananda Reddy, G.; Narasimha Murty, B.; Ravindra, H.R.

2013-01-01

One of the many routes of production of nuclear grade zirconium dioxide involve separation of zirconium and hafnium by solvent extraction of zirconium nitrate using tri-n-butyl phosphate followed by precipitation of zirconium with ammonia and finally calcination of the so obtained hydrated zirconia at elevated temperature. The zirconium feed solution as is generated from digestion of zirconium washed dried frit (produced by the caustic fusion of zircon sand which is one of the beach sand heavy minerals) in nitric acid contain considerable amount of sludge material and after solvent extraction this whole sludge material rests with raffinate. This sludge material has a scope to contain considerable amounts of zirconium along with other metal ions such as hafnium, aluminium, iron, etc. besides nitric acid and it constitutes one of the important solid wastes that needs to be disposed suitably. One of the disposal means of this sludge material is to use it as a land fill for which two important criteria are to be viz the pH of 10% solid waste solution should be near to neutral pH and the loss on ignition at 550℃ on dry basis of the sludge to be below 20%. In order to study the implications of presence of varying amounts of zirconium nitrate in the sludge on the pH of 10% solution of the sludge various synthetic zirconium nitrate solid waste were prepared using the sludge material generated at the laboratory during the analysis of zirconium washed dried frit. Presence of zirconium in the sludge is expected to decrease the overall pH of the 10% solution of the sludge because zirconium is prone to hydrolyze especially locally when zirconium ion comes into contact with water according to the chemical equation Zr 4+ H 2 O → ZrO 2+ + 2H + . From this equation, it is clear that for every one mole of zirconium ions two moles of hydrogen ions are produced. This is verified experimentally using the synthetically prepared sludge materials with varying amounts of zirconium

Solvent extraction of zirconium

International Nuclear Information System (INIS)

Kim, S.S.; Yoon, J.H.

1981-01-01

The extraction of zirconium(VI) from an aqueous solution of constant ionic strength with versatic acid-10 dissolved in benzen was studied as a function of pH and the concentration of zirconium(VI) and organic acid. The effects of sulphate and chlorine ions on the extraction of the zirconium(VI) were briefly examined. It was revealed that (ZrOR 2 .2RH) is the predominant species of extracted zirconium(VI) in the versatic acid-10. The chemical equation and the apparent equilibrium constants thereof have been determined as follows. (ZrOsup(2+))aq+ 2(R 2 H 2 )sub(org) = (ZrOR 2 .2RH)sub(org)+2(H + )aq Ksub(Zr) = (ZrOR 2 .2RH)sub(org)(H + ) 2 /(ZrOsup(2+))sub(aq)(R 2 H 2 )sup(2)sub(org) = 3.3 x 10 -7 . The synergistic effects of TBP and D2EHPA were also studied. In the mixed solvent with 0.1M TBP, the synergistic effect was observed, while the mixed solvent with D2EHPA showed the antisynergistic effect. (Author)

A study of a production process for hafnium-free zirconium from zircon

International Nuclear Information System (INIS)

Ratanalert, N.

1985-01-01

The purpose of this experiment was to extract and purify the zirconium from zircon. The effects of time of extraction and stripping of zirconium, concentration of feed solution, concentration of hydrochloric acid in stripping process, equilibrium curve of extraction of zirconium and hafnium and equilibrium curve of stripping zirconium or scrubbing hafnium were studied from standard zirconium and hafnium. The results, subsequently were applied to the extraction procedures for zirconium from zircon. Minus 100 mesh zircon was fused with sodium hydroxide in the ratio of 1 : 6 at 700 degree C for l hour. After fusion the zirconate was leached with water and dissolved in hot concentrated hydrochloric acid. Zirconyl chloride octahydrate crystallized out when the solution was cooled. An agueons solution of zirconyl chloride was used as the feed to the hexone - thiocyanate solvent extraction process. This was prepared by dissolving zirconyl chloride octahydrate crystal in waster. This zirconium feed solution in 1 M HCl and 1 M N H 4 CNS was extracted with 2.7 m N H 4 CNS in hexone and then stripped with 3.6 M HCl the aqueous phase was got rid of thiocyanate ion by extracting with pure hexone, then the zirconium in aqueous phase was precipitated with sulfuric acid and ammonium hydroxide at pH 1.8 - 2.0 and zirconium oxide was obtained by ignition at 700 degree C. The process could be modified to improve the purity of zirconium by using cation exchange resin to get rid of thiocyanate ion after solvent extraction process

Idaho chemical programs annual technical report, fiscal year 1974

International Nuclear Information System (INIS)

Bower, J.R.

1975-01-01

The operating experience in fuel processing, waste calcining, and other waste management activities for FY 1974 is summarized. A new zirconium fuel dissolver has performed well, and the first-cycle extraction system shows near-zero losses. Technical support activities include: a flowsheet to reduce acid consumption and volume of liquid wastes in the electrolytic process; a new dissolution process for ternary oxide PWR fuel using zirconium-fluoride-nitric acid dissolvent; a study and recommendation for treatment of fuel storage basin water; progress in design and development of processes for Rover and HTGR fuels, corrosion evaluation of bins containing calcined wastes showing corrosion rates indicative of a safe 500-year or greater storage life; demonstration on a pilot-plant scale of conditions for calcination of stainless steel and Rover fuel wastes as well as commercial wastes; evaluation of equipment alternatives for a new waste calcining facility; studies related to improvements in rare gas recovery and process off-gas treatment; demonstration of stability when various high-level waste solutions are mixed; progress on postcalcination treatment of calcined waste solids (ceramic formation, incorporation in metals, and calcine-concretes); studies on removal of actinides from ICPP wastes; a conceptual design for a proposed radioactive solid-waste repackaging facility for the INEL. Significant progress is reported on the program for determination of burnup for fast breeder reactor fuels. (U.S.)

Separation of sup(99m)Tc from 99Mo through a hydrous zirconium oxide column

International Nuclear Information System (INIS)

Mengatti, J.

1980-01-01

The preparation of 99 Mo-,sup(99m)Tc generator based on the adsorption of 99 Mo on hydrous zirconium oxide column, employing the in exchange technique, is described. The adsorption of 99 Mo on hydrous zirconium oxide (HZO) and the separation of sup(99m)Tc, generated by the decay of 99 Mo with saline solution, are analised. The sup(99m)Tc separation yield, pH of the eluted solution, aspect of the elution curve and the adsorption of 99 Mo on hydrous zirconium oxide calcined at 800 0 C are studied. The chemical and radioactive purities of the final product are analysed and the variation of the elution yield for successive elutions is studied. (Author) [pt

Study of some properties of zirconium phosphate

International Nuclear Information System (INIS)

Prospert, J.

1963-05-01

Zirconium phosphate has been studied with a view to using it as an ion exchanger: the first objective was to develop a method of preparation easy to apply and also reproducible. To this end, several tests were carried out varying the molar ratios of phosphorus and of zirconium. Some physical properties such as the diffraction of X-rays were examined. The work then involved certain chemical properties, particularly the percentages of free water and structural water given by the loss on calcination, the Karl-Fisher method and the weight losses by thermogravimetry. Finally an attempts was made to apply the exchanger to the separation of alkaline ions. The static tests showed that the order of fixation of these ions was Cs + > Rb + >> K + > Na + . Tests with columns showed that Na + and K + were easily separable, as was the Rb + -Cs + mixture, this last pair being fairly difficult to dissociate. (author) [fr

Fabrication of NiO/zirconium oxide nanofibers by electrospinning

Energy Technology Data Exchange (ETDEWEB)

Sundarrajan, Subramanian, E-mail: sundarnus1@gmail.com [Department of Mechanical Engineering, NUS, 117576 (Singapore); Venkatesan, Arunachalam; Agarwal, Satya R.; Shaik Anwar Ahamed, Nabeela Nasreen [Department of Mechanical Engineering, NUS, 117576 (Singapore); Ramakrishna, Seeram, E-mail: seeram@nus.edu.sg [Department of Mechanical Engineering, NUS, 117576 (Singapore); King Saud University, Riyadh 11451 (Saudi Arabia); Institute of Materials Research and Engineering, 117602 (Singapore)

2014-12-01

The electrospinning technique has been used to fabricate 1D inorganic–organic composite nanofibers from solutions containing poly(vinyl alcohol) (PVA) and suitable aqueous precursors of nickel and zirconium ions. Upon calcination, nickel oxide/zirconia nanofibers retained the original morphological features of as-spun nanofibers. X-ray diffraction was used to identify the crystalline nature of the final product and analytical tools such as Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM) were employed to elucidate the pathway of ceramic phase formation and the systematic evolution of morphological features in the as-spun and calcined fibers. These fibers will find potential applications in biomedical field. - Highlights: • PVA/NiO/zirconia composite nanofibers were synthesized via electrospinning. • Green processing of nanofibers using only water as solvent. • Calcination of composite nanofibers to yield ceramic nanofibers. • High aspect ratio nanofibers with diameters 106 ± 25 nm • The application of these fibers as dental composites and bone tissue engineering.

Zirconium behaviour during electrorefining of actinide-zirconium alloy in molten LiCl-KCl on aluminium cathodes

Energy Technology Data Exchange (ETDEWEB)

Meier, R. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, Karlsruhe 76125 (Germany); Heidelberg University, Institute of Physical Chemistry, Im Neuenheimer Feld 253, Heidelberg 69120 (Germany); Souček, P., E-mail: Pavel.Soucek@ec.europa.eu [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, Karlsruhe 76125 (Germany); Malmbeck, R.; Krachler, M.; Rodrigues, A.; Claux, B.; Glatz, J.-P. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, Karlsruhe 76125 (Germany); Fanghänel, Th. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, Karlsruhe 76125 (Germany); Heidelberg University, Institute of Physical Chemistry, Im Neuenheimer Feld 253, Heidelberg 69120 (Germany)

2016-04-15

A pyrochemical electrorefining process for the recovery of actinides from metallic nuclear fuel based on actinide-zirconium alloys (An–Zr) in a molten salt is being investigated. In this process actinides are group-selectively recovered on solid aluminium cathodes as An–Al alloys using a LiCl–KCl eutectic melt at a temperature of 450 °C. In the present study the electrochemical behaviour of zirconium during electrorefining was investigated. The maximum amount of actinides that can be oxidised without anodic co-dissolution of zirconium was determined at a selected constant cathodic current density. The experiment consisted of three steps to assess the different stages of the electrorefining process, each of which employing a fresh aluminium cathode. The results indicate that almost a complete dissolution of the actinides without co-dissolution of zirconium is possible under the applied experimental conditions. - Highlights: • Recovery of actinides was shown by electrorefining of U/Pu–Zr alloys in LiCl–KCl. • Constant current density of 20 mA/cm{sup 2} is applied. • Most of the actinides were dissolved avoiding zirconium co-dissolution. • Deterioration of the deposit quality by a small amount of co-deposited Zr is not observed.

Electrochemical stripping determination of traces of copper, lead, cadmium and zinc in zirconium metal and zirconium dioxide

International Nuclear Information System (INIS)

Stulik, K.; Beran, P.; Dolezal, J.; Opekar, F.

1978-01-01

Procedures have been developed for the determination of copper, lead, cadmium and zinc in zirconium metal and zirconium dioxide, at concentrations of 1ppm or less. Zirconium metal was dissolved in sulphuric acid, and zirconium dioxide decomposed under pressure with hydrofluoric acid. Sample solutions were prepared in dilute sulphuric acid. For the stripping determination, the sample solution was either mixed with a complexing tartrate base electrolyte or the pre-electrolysis was carried out in acid solution, with the acid solution being exchanged for a pure base electrolyte (e.g. an acetate buffer) for the stripping step. The stripping step was monitored by d.c., differential pulse and Kalousek commutator voltammetry and the three methods were compared. A stationary mercury-drop electrode can generally be used for all the methods, whereas a mercury-film electrode is suitable only for the d.c. voltammetric determination of copper, lead and cadmium, as pulse measurements with films are poorly reproducible and the electrodes are easily damaged. The relative standard deviation does not exceed 20%. Some samples contained relatively large amounts of copper, which is best separated by electrodeposition on a platinum electrode. (author)

Optimization of the conditions for producing zirconia by the precipitation of basic zirconium sulfate

International Nuclear Information System (INIS)

Ricci, D.R.; Paschoal, J.O.A.

1988-01-01

The process of precipitation of the basic sulfate from zirconium oxychlorides solutions has been optimized in order to obtain zirconia of high purity as well as suitable for ceramic processing. The main parameters of this study were obtained from the determination of the pH and of the concentration of the initial oxychloride solution, of the sulfate/zirconium molar ratio and of the reaction temperature. The following experimental procedure has been carried out: a) reaction of each precipitate with ammonium hydroxide followed by drying at 150 0 -C / 5 h and calcination at 1000 0 C / 1 h, yielding the final product (zirconia) b) product characterization by means of spectrographic, X - ray fluorescence and diffractometry analyses, determination of grain size distribution and of apparent density, and morphology study by scanning electron microscopy. The yielding of the overall reaction has been determined by chemical analysis and the composition of the basic zirconium sulfate by thermogravimetric analyses. (author) [pt

Calcine production and management

International Nuclear Information System (INIS)

Dickey, B.R.; Hogg, G.W.; Berreth, J.R.

1979-01-01

The process technology related to calcination of power reactor wastes is summarized. The primary calcination processes developed are spray calcination, fluidized-bed calcination, and rotary kiln calcination. Calcines from the spray calciner and rotary kiln are fed directly to a glassification process. The fluidized-bed product can either be fed to a waste form conversion process or stored. The major process steps for calcinations are feed preparation, calcination and product handling, and off-gas cleanup. Feed systems for the three processes are basically similar. Gravity flow and pump pressurized systems have been used successfully. The major problems are fatigue failure of feed valve bellows, plugging by undissolved solids, and calibration of flowmeters. Process heat input is by electrical resistance heating for the spray and rotary kiln calciners and in-bed combustion or in-bed heat exchange for the fluidized-bed system. Low-melting solids which can cause scaling or solids agglomeration in any of the processes is a major calcination problem; however, feed blending, process operating conditions, and equipment design have successfully controlled solids agglomeration. Primary off-gas cleanup devices for particulates are cyclones, sintered metal filters, venturi scrubbers, and HEPA filters. Scrubbers, condensers, and solid adsorbents are used successfully for volatile ruthenium removal. The years of pilot-plant and plant-scale calcination testing and operation of the three systems have shown that reactor wastes can be calcined safely and practically. 11 figures, 2 tables

Methods for the preparation of ultra-pure anhydrous zirconium tetrafluoride from zirconium tetraborohydride, researches in connection with halide glasses

International Nuclear Information System (INIS)

Tortevois, R.

1990-01-01

The synthesis of ultrapure zirconium tetrafluoride, the main component of fluorozirconate based optical fibers, was successfully attempted from zirconium tetraborohydride. Of the fluorinating agents used, nitrogen trifluoride doesn't react with zirconium tetraborohydride while xenon difluoride reacts too violently and leads to phases which contain boron. The fluorination in a compatible solvent enabled us to minimize the degradation. The best results were obtained with the fluorination of Zr(BH 4 ) 4 dissolved in CFCl 3 at -40 deg C by anhydrous HF. Using several analytical methods such as graphite furnace atomic absorption and proton activation, we analyzed the purity. The degree of transition element impurities is less than the ppm level for ZrF 4 . The dehydration of ZrF 4 ,H 2 O and ZrF 4 ,3H 2 O at room temperature by CIF 3 in gaseous and liquid state was also investigated. At exceptionally low temperature, this process allows oxide and oxyfluoride components to be reduced

Chemistry of proposed calcination/dissolution processing of Hanford Site tank wastes

International Nuclear Information System (INIS)

Delegard, C.H.

1995-01-01

Plans exist to separate radioactive waste stored in underground tanks at the US Department of Energy's Hanford Site in south central Washington State into low-level and high-level fractions, and to immobilize the separate fractions in high-integrity vitrified forms for long-term disposal. Calcination with water dissolution has been proposed as a possible treatment for achieving low/high-level separation. Chemistry development activities conducted since 1992 with simulated and genuine tank waste show that calcination/dissolution destroys organic carbon and converts nitrate and nitrite to hydroxide and benign offgases. The process also dissolves significant quantities of bulk chemicals (aluminum, chromium, and phosphate), allowing their redistribution from the high-level to the low-level fraction. Present studies of the chemistry of calcination/dissolution processing of genuine wastes, conducted in the period October 1993 to September 1994, show the importance of sodium fluoride phosphate double salt in controlling phosphate dissolution. Peptization of waste solids is of concern if extensive washing occurs. Strongly oxidizing conditions imposed by calcination reactions were found to convert transition metals to soluble anions in the order chromate > manganate > > ferrate. In analogy with manganese behavior, plutonium dissolution, presumably by oxidation to more soluble anionic species, also occurs by calcination/dissolution. Methods to remove plutonium from the product low-level solution stream must be developed

Zirconium oxide crystal phase: The role of the pH and time to attain the final pH for precipitation of the hydrous oxide

International Nuclear Information System (INIS)

Srinivasan, R.; Harris, M.B.; Simpson, S.F.; De Angelis, R.J.; Davis, B.H.

1988-01-01

Precipitated hydrous zirconium oxide can be calcined to produce either a monoclinic or tetragonal product. It has been observed that the time taken to attain the final pH of the solution in contact with the precipitate plays a dominant role in determining the crystal structure of the zirconium oxide after calcination at 500 0 C. The dependence of crystal structure on the rate of precipitation is observed only in the pH range 7--11. Rapid precipitation in this pH range yields predominately monoclinic zirconia, whereas slow (8 h) precipitation produces the tetragonal phase. At pH of approximately 13.0, only the tetragonal phase is formed from both slowly and rapidly precipitated hydrous oxide. The present results, together with earlier results, show that both the pH of the supernatant liquid and the time taken to attain this pH play dominant roles in determining the crystal structure of zirconia that is formed after calcination of the hydrous oxide. The factors that determine the crystal phase are therefore imparted in a mechanism of precipitation that depends upon the pH, and it is inferred that it is the hydroxyl concentration that is the dominant factor

Structural studies of calcium phosphate doped with titanium and zirconium obtained by high-energy mechanical alloying

Energy Technology Data Exchange (ETDEWEB)

Silva, C C; Sombra, A S B [Telecommunications and Materials Science and Engineering Laboratory (LOCEM), Physics Department, Federal University of Ceara, Campus do Pii, Postal Code 6030, 60455-760, Fortaleza-Ceara (Brazil)], E-mail: sombra@fisica.ufc.br

2009-12-15

In this paper, we present a new variation of the solid-state procedure on the synthesis of bioceramics with titanium (CapTi) and zirconium (CapZr), considering that zirconium (ZrO{sub 2}) and titanium oxide (TiO{sub 2}) are strengthening agents, due to their superb force and fracture toughness. The high efficiency of the calcination process opens a new way of producing commercial amounts of nanocrystalline bioceramics. In this work, a new variation of the solid-state procedure method was used to produce nanocrystalline powders of titanium and zirconium, using two different experimental chemical routes: CapTi: Ca(H{sub 2}PO{sub 4}){sub 2}+TiO{sub 2} and CapZr: Ca(H{sub 2}PO{sub 4}){sub 2}+ZrO{sub 2}. The powders were submitted to calcination processes (CapTic and CapZrc) at 800, 900 and 1000 deg. C. The calcium titanium phosphate phase, CaTi{sub 4}P{sub 6}O{sub 24}, was obtained in the CapTic reaction and the calcium zirconium phosphate, CaZr{sub 4}P{sub 6}O{sub 24}, was obtained in the CapZrc reaction. The obtained ceramics were characterized by x-ray powder diffraction (XRD), infrared (IR) spectroscopy, Raman scattering spectroscopy (RSS) and scanning electron microscopy (SEM) analysis. This method was compared with the milling process (CapTim and CapZrm), where in the last process the melting is not necessary and the powder obtained is nanocrystalline. The calcium titanium phosphate phase, CaTi{sub 4}P{sub 6}O{sub 24}, was obtained in the reaction CapTim, but in CapZrm the formation of any calcium phosphate phase even after 15 h of dry mechanical alloying was not observed.

Study of some properties of zirconium phosphate; Etude de quelques proprietes du phosphate de zirconium

Energy Technology Data Exchange (ETDEWEB)

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

1963-05-01

Zirconium phosphate has been studied with a view to using it as an ion exchanger: the first objective was to develop a method of preparation easy to apply and also reproducible. To this end, several tests were carried out varying the molar ratios of phosphorus and of zirconium. Some physical properties such as the diffraction of X-rays were examined. The work then involved certain chemical properties, particularly the percentages of free water and structural water given by the loss on calcination, the Karl-Fisher method and the weight losses by thermogravimetry. Finally an attempts was made to apply the exchanger to the separation of alkaline ions. The static tests showed that the order of fixation of these ions was Cs{sup +} > Rb{sup +} >> K{sup +} > Na{sup +}. Tests with columns showed that Na{sup +} and K{sup +} were easily separable, as was the Rb{sup +}-Cs{sup +} mixture, this last pair being fairly difficult to dissociate. (author) [French] Le phosphate de zirconium a ete etudie en vue de son utilisation comme echangeur d'ions: le premier but a atteindre a ete de mettre au point une preparation pouvant se reveler facilement utilisable ainsi qu'aisement reproductible. A cet effet, plusieurs essais ont ete effectues en faisant varier les rapports molaires du phosphore et du zirconium. Quelques proprietes physiques, telle la diffraction des rayons X, ont ete abordees. Ensuite, l'etude a porte sur certaines proprietes chimiques, particulierement les pourcentages d'eau libre et d'eau de structure par des pertes au feu, utilisation de la methode de Karl-Fisher, ainsi que des pertes de poids a la thenmobalance. Enfin, on a tente d'utiliser l'echangeur a la separation des ions alcalins. Les etudes statiques ont permis de constater que l'ordre de fixation de ces ions etait Cs{sup +} > Rb{sup +} >> K{sup +} > Na{sup +}. Les essais effectues en colonne ont montre que Na{sup +} et K{sup +} etaient aisement separables entre eux, ainsi que du couple Rb{sup +}-Cs{sup +}, ce

ENTIRELY AQUEOUS SOLUTION-GEL ROUTE FOR THE PREPARATION OF ZIRCONIUM CARBIDE, HAFNIUM CARBIDE AND THEIR TERNARY CARBIDE POWDERS

Directory of Open Access Journals (Sweden)

Zhang Changrui

2016-07-01

Full Text Available An entirely aqueous solution-gel route has been developed for the synthesis of zirconium carbide, hafnium carbide and their ternary carbide powders. Zirconium oxychloride (ZrOCl₂.8H₂O, malic acid (MA and ethylene glycol (EG were dissolved in water to form the aqueous zirconium carbide precursor. Afterwards, this aqueous precursor was gelled and transformed into zirconium carbide at a relatively low temperature (1200 °C for achieving an intimate mixing of the intermediate products. Hafnium and the ternary carbide powders were also synthesized via the same aqueous route. All the zirconium, hafnium and ternary carbide powders exhibited a particle size of ∼100 nm.

Methods for determination of zirconium in titanium alloys

International Nuclear Information System (INIS)

1985-01-01

Two methods for determining zirconium content in titanium alloys are specified in this standard. One is the ion-exchange/mandelic acid gravimetry for Zr content below 20 % down to 1 % while the other is the mandelic acid gravimetry for Zr content below 20 % down to 0.5 %. In the former, a specimen is decomposed by hydrochloric acid and hydrofluoric acid. After substances such as titanium are oxidized by adding nitric acid, the liquid is adjusted into a 4N hydrochloric acid - gN hydrofluoric acid solution, which is them passed through an ion-exchange column. The niobium and tantalum contents are absorbed while the titanium and zirconium contents flow out. Perchloric acid and sulfuric acid are poured in the solution to remove hydrofluoric acid. Aqueous ammonia is added to produce hydroxide of titanium and zirconium, which is then filtered out. The hydroxyde is dissolved in hydrochloric acid, and mandelic acid is poured to precipitate the zirconium content. The precipitate is ignited and the weight of the oxide formed is measured. The coprecipitated titanium content is determined by the absorptiometric method using hydrogen peroxide. Finally, the weight of the oxide is corrected. In the latter determination method, on the other hand, only several steps of the above procedure are used, namely, decomposition by hydrochloric acid, precipitation of zirconium, ignition of precipitate, measurement of oxide weight and weight correction. (Nogami, K.)

Spray calcination of nuclear wastes

International Nuclear Information System (INIS)

Bonner, W.F.; Blair, H.T.; Romero, L.S.

1976-01-01

The spray calciner is a relatively simple machine; operation is simple and is easily automated. Startup and shutdown can be performed in less than an hour. A wide variety of waste compositions and concentrations can be calcined under easily maintainable conditions. Spray calcination of all commercial fuel reprocessor high-level liquid wastes and mixed high and intermediate-level wastes have been demonstrated. Wastes have been calcined containing over 2M sodium. Thus waste generated during plant startup and shutdown can be blended with normal waste and calcined. Spray calcination of ILLW has also been demonstrated. A remotely replaceable atomizing nozzle has been developed for use in plant scale equipment. The 6 mm (0.25 inch) orifice and ceramic tip offer freedom from plugging and erosion thus nozzle replacement should be required only after several months operation. Calciner capacity of over 75 l/h (20 gal/h) has been demonstrated in pilot scale equipment. Sintered stainless steel filters are effective in deentraining over 99.9 percent of the solids that result from calcining the feedstock. Since such a small amount of radionuclides escape the calciner the volume of recycle required from the effluent treatment system is very small. The noncondensable off-gas volume is also low, less than 0.5 m 3 /min (15 scfm) for a liquid feedrate of 75 l/hr (20 gal/hr). Calcine holdup in the calciner is less than 1 kg, thus the liquid feedrate is directly relatable to calcine flowrate. The calcine produced is very fine and reactive. Successful remote operation and maintenance of a heated wall spray calciner has been demonstrated while processing actual high-level waste. During these operations radionuclide volatilization from the calciner was acceptably low. 8 figures

Arsenic removal from aqueous solutions by sorption onto zirconium- and titanium-modified sorbents

Directory of Open Access Journals (Sweden)

Ignjatović Ljubiša

2011-01-01

Full Text Available Arsenic reduction in drinking water can include treatment by adsorption, switching to alternative water sources, or blending with water that has a lower arsenic concentration. Commercial sorbents MTM, Greensand and BIRM (Clack Corporation were modified with zirconium and titanium after activation. The modifications were performed with titanium tetrachloride and zirconium tetrachloride. The modified sorbents were dried at different temperatures. The sorption of arsenate and arsenite dissolved in drinking water (200μg L-1 onto the sorbents were tested using a batch procedure. After removal of the sorbent, the concentration of arsenic was determined by HG-AAS. Zirconium-modified BIRM showed the best performance for the removal of both arsenite and arsenate. Modification of the greensand did not affect arsenic sorption ability. Zirconium-modified BIRM diminished the concentration of total As to below 5 μg L-1.

Structural and luminescence properties of europium(III)-doped zirconium carbonates and silica-supported Eu3+-doped zirconium carbonate nanoparticles

International Nuclear Information System (INIS)

Sivestrini, S.; Riello, P.; Freris, I.; Cristofori, D.; Enrichi, F.; Benedetti, A.

2010-01-01

The synthesis, morphology and luminescence properties of europium(III)-doped zirconium carbonates prepared as bulk materials and as silica-supported nanoparticles with differing calcination treatments are reported. Transmission electron microscopy and X-ray diffraction analyses have, respectively, been used to study the morphology and to quantify the atomic amount of europium present in the optically active phases of the variously prepared nanomaterials. Rietveld analysis was used to quantify the constituting phases and to determinate the europium content. Silica particles with an approximate size of 30 nm were coated with 2 nm carbonate nanoparticles, prepared in situ on the surface of the silica core. Luminescence measurements revealed the role of different preparation methods and of europium-doping quantities on the optical properties observed.

Calcination/dissolution residue treatment

International Nuclear Information System (INIS)

Knight, R.C.; Creed, R.F.; Patello, G.K.; Hollenberg, G.W.; Buehler, M.F.; O'Rourke, S.M.; Visnapuu, A.; McLaughlin, D.F.

1994-09-01

Currently, high-level wastes are stored underground in steel-lined tanks at the Hanford site. Current plans call for the chemical pretreatment of these wastes before their immobilization in stable glass waste forms. One candidate pretreatment approach, calcination/dissolution, performs an alkaline fusion of the waste and creates a high-level/low-level partition based on the aqueous solubilities of the components of the product calcine. Literature and laboratory studies were conducted with the goal of finding a residue treatment technology that would decrease the quantity of high-level waste glass required following calcination/dissolution waste processing. Four elements, Fe, Ni, Bi, and U, postulated to be present in the high-level residue fraction were identified as being key to the quantity of high-level glass formed. Laboratory tests of the candidate technologies with simulant high-level residues showed reductive roasting followed by carbonyl volatilization to be successful in removing Fe, Ni, and Bi. Subsequent bench-scale tests on residues from calcination/dissolution processing of genuine Hanford Site tank waste showed Fe was separated with radioelement decontamination factors of 70 to 1,000 times with respect to total alpha activity. Thermodynamic analyses of the calcination of five typical Hanford Site tank waste compositions also were performed. The analyses showed sodium hydroxide to be the sole molten component in the waste calcine and emphasized the requirement for waste blending if fluid calcines are to be achieved. Other calcine phases identified in the thermodynamic analysis indicate the significant thermal reconstitution accomplished in calcination

New Waste Calciner High Temperature Operation

International Nuclear Information System (INIS)

Swenson, M.C.

2000-01-01

A new Calciner flowsheet has been developed to process the sodium-bearing waste (SBW) in the INTEC Tank Farm. The new flowsheet increases the normal Calciner operating temperature from 500 C to 600 C. At the elevated temperature, sodium in the waste forms stable aluminates, instead of nitrates that melt at calcining temperatures. From March through May 2000, the new high-temperature flowsheet was tested in the New Waste Calcining Facility (NWCF) Calciner. Specific test criteria for various Calciner systems (feed, fuel, quench, off-gas, etc.) were established to evaluate the long-term operability of the high-temperature flowsheet. This report compares in detail the Calciner process data with the test criteria. The Calciner systems met or exceeded all test criteria. The new flowsheet is a visible, long-term method of calcining SBW. Implementation of the flowsheet will significantly increase the calcining rate of SBW and reduce the amount of calcine produced by reducing the amount of chemical additives to the Calciner. This will help meet the future waste processing milestones and regulatory needs such as emptying the Tank Farm

Electroless deposition process for zirconium and zirconium alloys

Science.gov (United States)

Donaghy, Robert E.; Sherman, Anna H.

1981-01-01

A method is disclosed for preventing stress corrosion cracking or metal embrittlement of a zirconium or zirconium alloy container that is to be coated on the inside surface with a layer of a metal such as copper, a copper alloy, nickel, or iron and used for holding nuclear fuel material as a nuclear fuel element. The zirconium material is etched in an etchant solution, desmutted mechanically or ultrasonically, oxidized to form an oxide coating on the zirconium, cleaned in an aqueous alkaline cleaning solution, activated for electroless deposition of a metal layer and contacted with an electroless metal plating solution. This method provides a boundary layer of zirconium oxide between the zirconium container and the metal layer.

Radiant-heat spray-calcination process for the solid fixation of radioactive waste. Part 1, Non-radioactive pilot unit

Energy Technology Data Exchange (ETDEWEB)

Allemann, R.T.; Johnson, B.M. Jr.

1960-11-14

The fixation of radioactive waste in a stable solid media by means of calcination of these aqueous solutions has been the subject of considerable-effort throughout the U. S. Atomic Energy Commission and by atomic energy organizations in other countries. Several methods of doing this on a continuous or semi-continuous basis have been devised, and a fev have been demonstrated to be feasible for the handling of non-radioactive, or low-activity, simulated wastes. Notable among methods currently under development are: (a) batch-operated pot calcination of waste generated from reprocessing stainless steel clad fuel elements (Darex process) and Purex waste, (b) combination rotary kiln and ball mill calcination of aluminum nitrate (TBP-25 and Redox process), and (c) fluidized bed calcination of TBP-25 and Purex wastes. Although a considerable amount of engineering experience has been obtained on the calcination of dissolved salts in a fluidized bed, and the other methods have been the subjects of a great deal of study, none of them have been developed to-the extent which would rule out the desirability of further investigation of other possible methods of calcination.

Method for calcining radioactive wastes

International Nuclear Information System (INIS)

Bjorklund, W.J.; McElroy, J.L.; Mendel, J.E.

1979-01-01

A method for the preparation of radioactive wastes in a low leachability form involves calcining the radioactive waste on a fluidized bed of glass frit, removing the calcined waste to melter to form a homogeneous melt of the glass and the calcined waste, and then solidifying the melt to encapsulate the radioactive calcine in a glass matrix

Use of the azeotropic distillation technique in the synthesis of zirconium post ceramics

International Nuclear Information System (INIS)

Ussui, V.; Lazar, D.R.R.; Menezes, F.; Menezes, C.A.B.; Paschoal, J.O.A.

1996-01-01

The azeotropic distillation technique has been used for treatment of coprecipitated zirconium and yttrium hydroxides, in order to synthesize weak agglomerated powders. Experiments were performed by preparing suspensions of this precipitate with organic solvents as toluene, isopropanol, butanol and ethanol, which were submitted to the distillation, to remove all the liquid phase. The obtained powders after drying and calcination, have been characterized by granulometric distribution and specific surface area determination. The densities of the ceramic bodies, obtained by pressing and sintering at 1500 deg C during 1 hour, have also been evaluated. (author)

Experimental and modeling study of flash calcination of kaolinite rich clay particles in a gas suspension calciner

DEFF Research Database (Denmark)

Gebremariam, Abraham Teklay; Yin, Chungen; Rosendahl, Lasse

2015-01-01

gas suspension calciner, with the aim to derive useful guidelines on smart calcination for obtaining products of the best pozzolanic properties. Calcination tests are performed in the calciner under six different operation conditions. The raw feed and the calcined clay samples are all characterized...

Study of variation grain size in desulfurization process of calcined petroleum coke

Science.gov (United States)

Pintowantoro, Sungging; Setiawan, Muhammad Arif; Abdul, Fakhreza

2018-04-01

Indonesia is a country with abundant natural resources, such as mineral mining and petroleum. In petroleum processing, crude oil can be processed into a source of fuel energy such as gasoline, diesel, oil, petroleum coke, and others. One of crude oil potentials in Indonesia is petroleum coke. Petroleum coke is a product from oil refining process. Sulfur reducing process in calcined petroleum cokes can be done by desulfurization process. The industries which have potential to become petroleum coke processing consumers are industries of aluminum smelting (anode, graphite block, carbon mortar), iron riser, calcined coke, foundry coke, etc. Sulfur reducing process in calcined petroleum coke can be done by thermal desulfurization process with alkaline substance NaOH. Desulfurization of petroleum coke process can be done in two ways, which are thermal desulfurization and hydrodesulphurization. This study aims to determine the effect of various grain size on sulfur, carbon, and chemical bond which contained by calcined petroleum coke. The raw material use calcined petroleum coke with 0.653% sulfur content. The grain size that used in this research is 50 mesh, then varied to 20 mesh and 100 mesh for each desulfurization process. Desulfurization are tested by ICP, UV-VIS, and FTIR to determine levels of sulfur, carbon, chemical bonding and sulfur dissolved water which contained in the residual washing of calcined petroleum coke. From various grain size that mentioned before, the optimal value is on 100 mesh grain size, where the sulfur content in petroleum coke is 0.24% and carbon content reaches the highest level of 97.8%. Meanwhile for grain size 100 mesh in the desulfurization process is enough to break the chemical bonds of organic sulfur in petroleum coke.

Summary of Waste Calcination at INTEC

Energy Technology Data Exchange (ETDEWEB)

O' Brien, Barry Henry; Newby, Bill Joe

2000-10-01

Fluidized-bed calcination at the Idaho Nuclear Technologies and Engineering Center (INTEC, formally called the Idaho Chemical Processing Plant) has been used to solidify acidic metal nitrate fuel reprocessing and incidental wastes wastes since 1961. A summary of waste calcination in full-scale and pilot plant calciners has been compiled for future reference. It contains feed compositions and operating conditions for all the processing campaigns for the original Waste Calcining Facility (WCF), the New Waste Calcining Facility (NWCF) started up in 1982, and numerous small scale pilot plant tests for various feed types. This summary provides a historical record of calcination at INTEC, and will be useful for evaluating calcinability of future wastes.

Zirconium-cerin solid solutions: thermodynamic model and thermal stability at high temperature; Solutions solides de zirconium dans la cerine: modele thermodynamique et stabilite thermique a haute temperature

Energy Technology Data Exchange (ETDEWEB)

Janvier, C.

1998-04-02

The oxides-gaseous dioxygen equilibria and the textural thermal stability of six zirconium-cerin solutions Ce{sub 1-x}Zr{sub x}O{sub 2} (0zirconium concentration. A kinetic study (by calcination at 950 degrees Celsius of the solid solutions) of the specific surface area decrease has revealed a minima (0

Corrosion behavior of stainless steel and zirconium in nitric acid containing highly oxidizing species

International Nuclear Information System (INIS)

Mayuzumi, Masami; Fujita, Tomonari

1994-01-01

Corrosion behavior of 304ELC, 310Nb stainless steels and Zirconium was investigated in the simulated dissolver solution of a reprocessing plant to obtain fundamental data for life prediction. Corrosion of heat transfer surface was also investigated in nitric acid solutions containing Ce ion. The results obtained are as follows: (1) Stainless steels showed intergranular corrosion in the simulated dissolver solution. The corrosion rate increased with time and reached to a constant value after several hundred hours of immersing time. The constant corrosion rate changed depending on potential suggesting that corrosion potential dominates the corrosion process. 310Nb showed superior corrosion resistance to 304ELC. (2) Corrosion rate of stainless steels increased in the heat transfer condition. The causes of corrosion enhancement are estimated to be higher corrosion potential and higher temperature of heat transfer surface. (3) Zirconium showed perfect passivity in all the test conditions employed. (author)

Estimation of niobium, tantalum and zirconium in a carbonate rich ore

International Nuclear Information System (INIS)

Navale, A.S.; Venkatakrishnan, R.R.; Sreenivas, T.

2013-01-01

Tantalum, niobium and zirconium form refractory compounds and therefore pose problems in estimation by methods like spectrophotometry, AAS etc. Their estimation is best carried out with ICP-OES as the plasma is capable of breaking the refractory compounds and releases these elements in the form of excited atoms. But another major problem is bringing these elements in solution as they require very strong reagents and tend to hydrolyze easily in solution. Complexing agents need to be added to maintain these elements in dissolved condition. The commonly employed dissolution techniques for these elements are fusion with potassium pyrosulfate (for Nb and Ta), sodium hydroxide or peroxide (for zirconium). Digestion with mineral acids in combination with hydrofluoric acid is also employed

Effect of Sol Concentration, Aging and Drying Process on Cerium Stabilization Zirconium Gel Produced by External Gelation

Science.gov (United States)

Sukarsono, R.; Rachmawati, M.; Susilowati, S. R.; Husnurrofiq, D.; Nurwidyaningrum, K.; Dewi, A. K.

2018-02-01

Cerium Stabilized Zirconium gel has been prepared using external gelation process. As the raw materials was used ZrO(NO3)2 and Ce(NO3)4 nitrate salt which was dissolved with water into Zr-Ce nitrate mixture. The concentration of the nitrate salt mixture in the sol solution was varied by varying the concentration of zirconium and cerium nitrate in the sol solution and the addition of PVA and THFA to produce a sol with a viscosity of 40-60 cP. The viscosity range of 40-60cP is the viscosity of the sol solution that was easy to produce a good gel in the gelation apparatus. Sol solution was casted in a gelation column equipped with following tools: a 1 mm diameter drip nozzle which was vibrated to adjust the best frequency and amplitude of vibration, a flow meter to measure the flow rate of sol, flowing of NH3 gas to presolidification process. Gelation column was contained NH4OH solution as gelation medium and gel container to collect gel product. Gel obtained from the gelation process than processed with ageing, washing, drying and calcinations to get round gel and not broken at calcinations up to 500°C. The parameters observed in this research are variation of Zr nitrate concentration, Ce nitrate concentration, ratio of Zr and Ce in the sol and ageing and drying process method which was appropriate to get a good gel. From the gelation processes that has been done, it can be seen that with the presolidification process can be obtained a round gel and without presolidification process, produce not round gel. In the process of ageing to get not broken gel, ageing was done on the rotary flask so that during the ageing, gels rotate in gelation media. Gels, then be washed by dilute ammonium nitrate, demireralized water and iso prophyl alcohol. The washed gel was then dried by vacuum drying to form pores on the gel which become the path for the gases resulting from decomposition of the gel to exit the gel. Vacuum drying can prevent cracking because the pores allow the gel

Effect of ultrasound on the structural and textural properties of copper-impregnated cerium-modified zirconium-pillared bentonite

International Nuclear Information System (INIS)

Tomul, Fatma

2011-01-01

In this study, the synthesis of zirconium-pillared bentonite modified with cerium was performed via two different methods by the application of conventional and ultrasonic treatments during the intercalation stage. To synthesise copper-impregnated pillared clays by wet impregnation, cerium-modified zirconium-pillared clays were used as supportive materials after being calcined at 300 °C. Ultrasonic treatment significantly decreased the required processing time compared with the conventional treatment of the synthesised pillared bentonites. Chemical analysis confirmed the incorporation of Zr 4+ , Ce 4+ and Cu 2+ species into the pillared bentonites. X-ray diffraction (XRD) patterns of zirconium- and cerium/zirconium-pillared bentonites prepared by conventional treatment show that one large d-spacing above 3.5 nm corresponds to the mesoporous delaminated part, and another small d-spacing above 1.7 nm is indicative of the microporous pillared part. Zirconium- and cerium/zirconium-pillared bentonites prepared via ultrasonic treatment exhibited similar results, with the same high d-spacing but with a second low-intensity d-spacing above 1.9 nm. The delaminated structures of the pillared bentonites synthesised by both methods were conserved after copper impregnation. Nitrogen-adsorption isotherm analysis showed that the textural characteristics of products synthesised by ultrasonic treatment were comparable to those of products synthesised by conventional treatment. Fourier-transform infrared spectroscopy (FTIR) analyses showed the presence of Brønsted- and Lewis-acid sites, and zirconium-pillared clays synthesised by conventional treatment exhibited increased numbers of Brønsted- and Lewis-acid sites after cerium addition and copper impregnation. However, the products synthesised by ultrasonic treatment exhibited an increased number of Brønsted- and Lewis-acid sites after cerium addition, but a decreased number of acid sites after copper impregnation.

Alternative calcination development status report

International Nuclear Information System (INIS)

Boardman, R.D.

1997-12-01

The Programmatic Spent Nuclear Fuel and (INEEL) Environmental Restoration and Waste Management Programs Environmental Impact Statement Record of Decision, dated June 1, 1995, specifies that high-level waste stored in the underground tanks at the ICPP continue to be calcined while other options to treat the waste are studied. Therefore, the High-Level Waste Program has funded a program to develop new flowsheets to increase the liquid waste processing rate. Simultaneously, a radionuclide separation process, as well as other options, are also being developed, which will be compared to the calcination treatment option. Two alternatives emerged as viable candidates; (1) elevated temperature calcination (also referred to as high temperature calcination), and (2) sugar-additive calcination. Both alternatives were determined to be viable through testing performed in a lab-scale calcination mockup. Subsequently, 10-cm Calciner Pilot Plant scoping tests were successfully completed for both flowsheets. The results were compared to the standard 500 C, high-ANN flow sheet (baseline flowsheet). The product and effluent streams were characterized to help elucidate the process chemistry and to investigate potential environmental permitting issues. Several supplementary tests were conducted to gain a better understanding of fine-particles generation, calcine hydration, scrub foaming, feed makeup procedures, sugar/organic elimination, and safety-related issues. Many of the experiments are only considered to be scoping tests, and follow-up experiments will be required to establish a more definitive understanding of the flowsheets. However, the combined results support the general conclusion that flowsheet improvements for the NWCF are technically viable

Flash calcination of kaolinite rich clay and impact of process conditions on the quality of the calcines

DEFF Research Database (Denmark)

Gebremariam, Abraham Teklay; Yin, Chungen; Rosendahl, Lasse

2016-01-01

Use of properly calcined kaolinite rich clay (i.e., metakaolin) to offset part of CO2-intensive clinkers not only reduces CO2 footprint from cement industry but also improves the performance of concrete. However, calcination under inappropriately high temperatures or long retention times may...... suspension calciner. The model is validated by the experimental data (e.g., the degree of dehydroxylation and the density of the calcines). Based on the model, the impacts of process conditions and feed properties on the quality of the calcination products are thoroughly examined....

Hydrogen desorption kinetics from zirconium hydride and zirconium metal in vacuum

International Nuclear Information System (INIS)

Hu, Xunxiang; Terrani, Kurt A.; Wirth, Brian D.

2014-01-01

The kinetics of hydrogen desorption from zirconium hydride is important in many nuclear design and safety applications. In this paper, a coordinated experimental and modeling study has been used to explicitly demonstrate the applicability of existing kinetic theories for hydrogen desorption from zirconium hydride and α-zirconium. A static synthesis method was used to produce δ-zirconium hydride, and the crystallographic phases of the zirconium hydride were confirmed by X-ray diffraction (XRD). Three obvious stages, involving δ-zirconium hydride, a two-phase region, and α-zirconium, were observed in the hydrogen desorption spectra of two zirconium hydride specimens with H/Zr ratios of 1.62 and 1.64, respectively, which were obtained using thermal desorption spectroscopy (TDS). A continuous, one-dimensional, two-phase moving boundary model, coupled with the zero- and second-order kinetics of hydrogen desorption from δ-zirconium hydride and α-zirconium, respectively, has been developed to reproduce the TDS experimental results. A comparison of the modeling predictions with the experimental results indicates that a zero-order kinetic model is valid for description of hydrogen flux away from the δ-hydride phase, and that a second-order kinetic model works well for hydrogen desorption from α-Zr if the activation energy of desorption is optimized to be 70% of the value reported in the literature

Generalized Test Plan for the Vitrification of Simulated High-Level -Waste Calcine in the Idaho National Laboratory's Bench -Scale Cold Crucible Induction Melter

International Nuclear Information System (INIS)

Maio, Vince

2011-01-01

relatively high concentrations of zirconium and aluminum, representative of the cladding material of the reprocessed fuel that generated the calcine. A separate study to define the CCIM testing needs of these other calcine classifications in currently being prepared under a separate work package (WP-0) and will be provided as a milestone report at the end of this fiscal year.

In situ Raman Spectroscopy of Oxide Films on Zirconium Alloy in Simulated PWR Primary Water Condition

Energy Technology Data Exchange (ETDEWEB)

Kim, Tae Ho; Choi, Kyoung Joon; Yoo, Seung Chang; Kim, Ji Hyun [UNIST, Ulsan (Korea, Republic of)

2016-05-15

The two layered oxide structure is formed in pre-transition oxide for the zirconium alloy in high temperature water environment. It is known that the corrosion rate is related to the volume fraction of zirconium oxide and the pores in the oxides; therefore, the aim of this paper is to investigate the oxidation behavior in the pretransition zirconium oxide in high-temperature water chemistry. In this work, Raman spectroscopy was used for in situ investigations for characterizing the phase of zirconium oxide. In situ Raman spectroscopy is a well-suited technique for investigating in detail the characteristics of oxide films in a high-temperature corrosion environment. In previous studies, an in situ Raman system was developed for investigating the oxides on nickel-based alloys and low alloy steels in high-temperature water environment. Also, the early stage oxidation behavior of zirconium alloy with different dissolved hydrogen concentration environments in high temperature water was treated in the authors' previous study. In this study, a specific zirconium alloy was oxidized and investigated with in situ Raman spectroscopy for 100 d oxidation, which is close to the first transition time of the zirconium alloy oxidation. The ex situ investigation methods such as transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS) were used to further characterize the zirconium oxide structure. As oxidation time increased, the Raman peaks of tetragonal zirconium oxide were merged or became weaker. However, the monoclinic zirconium oxide peaks became distinct. The tetragonal zirconium oxide was just found near the O/M interface and this could explain the Raman spectra difference between the 30 d result and others.

Uranium dioxide calcining apparatus

International Nuclear Information System (INIS)

Cole, E.A.; Peterson, R.S.

1978-01-01

This invention relates to an improved continuous calcining apparatus for consistently and controllably producing from calcinable reactive solid compounds of uranium, such as ammonium diuranate, uranium dioxide (UO 2 ) having an oxygen to uranium ratio of less than 2.2. The apparatus comprises means at the outlet end of a calciner kiln for receiving hot UO 2 , means for cooling the UO 2 to a temperature of below 100 deg C and conveying the cooled UO 2 to storage or to subsequent UO 2 processing apparatus where it finally comes into contact with air, the means for receiving cooling and conveying being sealed to the outlet end of the calciner and being maintained full of UO 2 and so operable as to exclude atmospheric oxygen from coming into contact with any UO 2 which is at elevated temperatures where it would readily oxidize, without the use of extra hydrogen gas in said means. (author)

Properties of radioactive calcine retrieved from the second calcined solids storage facility at ICPP

International Nuclear Information System (INIS)

Staples, B.A.; Pomiak, G.S.; Wade, E.L.

1979-03-01

The chemical and physical properties of radioactive alumina and zirconia calcine samples retrieved from the storage bins at ICPP were measured. Chemical properties measured include chemical composition, crystalline structure, and radiochemical composition. The physical properties measured and reported include density, size distribution, relative attrition, solubility in 8 M HNO 3 , thermal stability, and flow characteristics. The chemical and physical properties of the retrieved calcine after the 10 to 12 years of storage are very similar to freshly prepared simulated calcine

Precipitation of γ-zirconium hydride in zirconium

International Nuclear Information System (INIS)

Carpenter, G.J.C.

1978-01-01

A mechanism for the precipitation of γ-zirconium hydride in zirconium is presented which does not require the diffusion of zirconium. The transformation is completed by shears caused by 1/3 (10 anti 10) Shockley partial dislocations on alternate zirconium basal planes, either by homogeneous nucleation or at lattice imperfections. Homogeneous nucleation is considered least likely in view of the large nucleation barrier involved. Hydrides may form at dislocations by the generation of partials by means of either a pole or ratchet mechanism. The former requires dislocations with a component of Burgers vector along the c-axis, but contrast experiments show that these are not normally observed in annealed zirconium. It is therefore most likely that intragranular hydrides form at the regular 1/3 (11 anti 20) dislocations, possibly by means of a ratchet mechanism. Contrast experiments in the electron microscope show that the precipitates have a shear character consistent with the mechanism suggested. The possibility that the shear dislocations associated with the hydrides are emissary dislocations is considered and a model suggested in which this function is satisfied together with the partial relief of misfit stresses. The large shear strains associated with the precipitation mechanism may play an important role in the preferential orientation of hydrides under stress

Structural and microstructural changes in the zirconium-indium mixed oxide system during the thermal treatment

Science.gov (United States)

Štefanić, G.; Štefanić, I. I.; Musić, S.; Ivanda, M.

2011-05-01

The zirconium-indium mixed oxide systems on both the zirconium- and the indium-rich side of the concentration range were prepared by co-precipitation from aqueous solutions of the corresponding salts, followed by washing and heat-treatment. The thermal behavior (up to 1000 °C) of the dried samples was examined by X-ray powder diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, energy dispersive X-ray spectrometry, differential thermal analysis and thermogravimetric measurements. The obtained results show that the increase in the amount of the second phase causes an increase of both the crystallization temperature of the amorphous precursors of ZrO 2, from 435 °C (0 mol.% of InO 1.5) to 476 °C (˜62 mol.% of InO 1.5), and of the topotactic transition temperature of cubic In(OH) 3 to cubic In 2O 3, from 259 °C (0 mol.% of ZrO 2) to 290 °C (˜25 mol.% of ZrO 2). The amorphous precursors of ZrO 2 phase exhibit an extended capability to incorporate In 3+ ions (more than 60 mol.%). With a rise in temperature the maximum solubility of In 3+ ions in the ZrO 2 lattice decreases from ˜55 mol.% in the crystallization products obtained after calcination at 400 °C to ˜10 mol.% after calcination at 1000 °C. The results of phase analysis indicate that the incorporation of In 3+ ions partially stabilized both the tetragonal and cubic ZrO 2 polymorphs. The maximum solubility of Zr 4+ ions in the starting In(OH) 3 lattice was estimated at ˜10 mol.%. Thermal treatment causes a small increase of Zr 4+ ion solubility limits, estimated at ˜15 mol.% in the cubic In 2O 3 lattice after calcination at 1000 °C. Precise lattice parameter measurements, by using Le Bail refinements of the powder diffraction patterns with added silicon as an internal standard, show that the incorporation of In 3+ ions caused a very small decrease of the cubic ZrO 2 lattice, while the incorporation of Zr 4+ ions had a negligible

Remotely replaceable fuel and feed nozzles for the new waste calcining facility calciner vessel

International Nuclear Information System (INIS)

Fletcher, R.D.; Carter, J.A.; May, K.W.

1978-01-01

The development and testing of remotely replaceable fuel and feed nozzles for calcination of liquid radioactive wastes in the calciner vessel of the New Waste Calcining Facility being built at the Idaho National Engineering Laboratory is described. A complete fuel nozzle assembly was fabricated and tested at the Remote Maintenance Development Facility to evolve design refinements, identify required support equipment, and develop handling techniques. The design also provided for remote replacement of the nozzle support carriage and adjacent feed and fuel pipe loops using two pairs of master-slave manipulators

Calcined solids storage facility closure study

International Nuclear Information System (INIS)

Dahlmeir, M.M.; Tuott, L.C.; Spaulding, B.C.

1998-02-01

The disposal of radioactive wastes now stored at the Idaho National Engineering and Environmental Laboratory is currently mandated under a open-quotes Settlement Agreementclose quotes (or open-quotes Batt Agreementclose quotes) between the Department of Energy and the State of Idaho. Under this agreement, all high-level waste must be treated as necessary to meet the disposal criteria and disposed of or made road ready to ship from the INEEL by 2035. In order to comply with this agreement, all calcined waste produced in the New Waste Calcining Facility and stored in the Calcined Solids Facility must be treated and disposed of by 2035. Several treatment options for the calcined waste have been studied in support of the High-Level Waste Environmental Impact Statement. Two treatment methods studied, referred to as the TRU Waste Separations Options, involve the separation of the high-level waste (calcine) into TRU waste and low-level waste (Class A or Class C). Following treatment, the TRU waste would be sent to the Waste Isolation Pilot Plant (WIPP) for final storage. It has been proposed that the low-level waste be disposed of in the Tank Farm Facility and/or the Calcined Solids Storage Facility following Resource Conservation and Recovery Act closure. In order to use the seven Bin Sets making up the Calcined Solids Storage Facility as a low-level waste landfill, the facility must first be closed to Resource Conservation and Recovery Act (RCRA) standards. This study identifies and discusses two basic methods available to close the Calcined Solids Storage Facility under the RCRA - Risk-Based Clean Closure and Closure to Landfill Standards. In addition to the closure methods, the regulatory requirements and issues associated with turning the Calcined Solids Storage Facility into an NRC low-level waste landfill or filling the bin voids with clean grout are discussed

Calcined solids storage facility closure study

Energy Technology Data Exchange (ETDEWEB)

Dahlmeir, M.M.; Tuott, L.C.; Spaulding, B.C. [and others

1998-02-01

The disposal of radioactive wastes now stored at the Idaho National Engineering and Environmental Laboratory is currently mandated under a {open_quotes}Settlement Agreement{close_quotes} (or {open_quotes}Batt Agreement{close_quotes}) between the Department of Energy and the State of Idaho. Under this agreement, all high-level waste must be treated as necessary to meet the disposal criteria and disposed of or made road ready to ship from the INEEL by 2035. In order to comply with this agreement, all calcined waste produced in the New Waste Calcining Facility and stored in the Calcined Solids Facility must be treated and disposed of by 2035. Several treatment options for the calcined waste have been studied in support of the High-Level Waste Environmental Impact Statement. Two treatment methods studied, referred to as the TRU Waste Separations Options, involve the separation of the high-level waste (calcine) into TRU waste and low-level waste (Class A or Class C). Following treatment, the TRU waste would be sent to the Waste Isolation Pilot Plant (WIPP) for final storage. It has been proposed that the low-level waste be disposed of in the Tank Farm Facility and/or the Calcined Solids Storage Facility following Resource Conservation and Recovery Act closure. In order to use the seven Bin Sets making up the Calcined Solids Storage Facility as a low-level waste landfill, the facility must first be closed to Resource Conservation and Recovery Act (RCRA) standards. This study identifies and discusses two basic methods available to close the Calcined Solids Storage Facility under the RCRA - Risk-Based Clean Closure and Closure to Landfill Standards. In addition to the closure methods, the regulatory requirements and issues associated with turning the Calcined Solids Storage Facility into an NRC low-level waste landfill or filling the bin voids with clean grout are discussed.

[Infrared spectral analysis for calcined borax].

Science.gov (United States)

Zhao, Cui; Ren, Li-Li; Wang, Dong; Zhou, Ping; Zhang, Qian; Wang, Bo-Tao

2011-08-01

To valuate the quality of calcined borax which is sold in the market, 18 samples of calcined borax were studied using the Fourier transform infrared, and samples with different water content were selected and analyzed. Then, the results of analysis were used to evaluate the quality of calcined borax. Results show that the infrared spectra of calcined borax include OH vibration, BO3(-3) vibration and BO4(5-) vibration absorption bands. The position and width of OH vibration absorption band depend on the level of water content, and the more the water content, the wider the absorption band. The number of BO3(3-) vibration and BO4(5-) vibration bands also depend on the level of water content, and the more the water content, and the stronger the hydrogen bond and the lower the symmetry of B atoms, the more the number of infrared absorption peaks. It was concluded that because the quality of calcined borax has direct correlation with water content, the infrared spectroscopy is an express and objective approach to quality analysis and evaluation of calcined borax.

Automatic measuring system of zirconium thickness for zirconium liner cladding tubes

International Nuclear Information System (INIS)

Matsui, K.; Yamaguchi, H.; Hiroshima, T.; Sakamoto, T.; Murayama, R.

1985-01-01

An automatic system of pure zirconium liner thickness for zirconium-zircaloy cladding tubes has been successfully developed. The system consists of three parts. (1) An ultrasonic thickness measuring method for mother tubes before cold rolling. (2) An electromagnetic thickness measuring method for the manufactured tubes. (3) An image processing method for the cross sectional view of the manufactured cut tube samples. In Japanese nuclear industry, zirconium-zircaloy cladding tubes have been tested in order to realize load following operation in the atomic power plant. In order to provide for the practical use in the near future, Sumitomo Metal Industries, Ltd. has been studied and established the practical manufacturing process of the zirconium liner cladding tubes. The zirconium-liner cladding tube is a duplex tube comprising an inner layer of pure zirconium bonded to zircaloy metallurgically. The thickness of the pure zirconium is about 10 % of the total wall thickness. Several types of the automatic thickness measuring methods have been investigated instead of the usual microscopic viewing method in which the liner thickness is measured by the microscopic cross sectional view of the cut tube samples

Zirconium and hafnium

Science.gov (United States)

Jones, James V.; Piatak, Nadine M.; Bedinger, George M.; Schulz, Klaus J.; DeYoung,, John H.; Seal, Robert R.; Bradley, Dwight C.

2017-12-19

Zirconium and hafnium are corrosion-resistant metals that are widely used in the chemical and nuclear industries. Most zirconium is consumed in the form of the main ore mineral zircon (ZrSiO4, or as zirconium oxide or other zirconium chemicals. Zirconium and hafnium are both refractory lithophile elements that have nearly identical charge, ionic radii, and ionic potentials. As a result, their geochemical behavior is generally similar. Both elements are classified as incompatible because they have physical and crystallochemical properties that exclude them from the crystal lattices of most rock-forming minerals. Zircon and another, less common, ore mineral, baddeleyite (ZrO2), form primarily as accessory minerals in igneous rocks. The presence and abundance of these ore minerals in igneous rocks are largely controlled by the element concentrations in the magma source and by the processes of melt generation and evolution. The world’s largest primary deposits of zirconium and hafnium are associated with alkaline igneous rocks, and, in one locality on the Kola Peninsula of Murmanskaya Oblast, Russia, baddeleyite is recovered as a byproduct of apatite and magnetite mining. Otherwise, there are few primary igneous deposits of zirconium- and hafnium-bearing minerals with economic value at present. The main ore deposits worldwide are heavy-mineral sands produced by the weathering and erosion of preexisting rocks and the concentration of zircon and other economically important heavy minerals, such as ilmenite and rutile (for titanium), chromite (for chromium), and monazite (for rare-earth elements) in sedimentary systems, particularly in coastal environments. In coastal deposits, heavy-mineral enrichment occurs where sediment is repeatedly reworked by wind, waves, currents, and tidal processes. The resulting heavy-mineral-sand deposits, called placers or paleoplacers, preferentially form at relatively low latitudes on passive continental margins and supply 100 percent of

Solvent extraction of titanium(IV), zirconium(IV) and hafnium(IV) salicylates using liquid ion exchangers

Energy Technology Data Exchange (ETDEWEB)

Sundaramurthi, N M; Shinde, V M

1989-02-01

A solvent extraction method is proposed for the extraction of quadrivalent titanium, zirconium an hafnium from salicylate media using liquid ion exchangers such as Aliquat 336 and trioctylamine dissolved in xylene. The optimum conditions were evaluated from a critical study of the following: pH, salicylate concentration, amine concentration, diluent and period of equilibration. The method allows the separation of titanium, zirconium and hafnium from binary mixtures containing commonly associated metal ions and is applicable to the analysis of real samples such as BCS-CRM 387 nimonic 901, BCS-CRM 243/4 ferro-titanium, BCS-CRM 307 magnesium alloy and BCS-CRM 388 zircon. Titanium is determined either with hydrogen peroxide or by atomic absorption spectrometry whereas zirconium and hafnium are determined spectrophotometrically with Alizarin Red S and Zylenol Orange, respectively. The results of both separation and analysis are reported. The method is precise, accurate and fast.

Radiochemical neutron activation analysis of zirconium and zirconium-niobium alloys

International Nuclear Information System (INIS)

Tashimova, F.A.; Sadikov, I.I.; Salimov, M.

2004-01-01

Full text: Zirconium and zirconium-niobium alloys are used on nuclear technology, as fuel cladding of nuclear reactors. Their nuclear-physical, mechanical and thermophysical properties are influenced them matrix and impurity composition, therefore determination of matrix and impurity content of these materials is a very important task. Neutron activation analysis is one from multielemental and high sensible techniques that are widely applied in analysis of high purity materials. Investigation of nuclear-physical characteristics of zirconium has shown that instrumental variant NAA is unusable for analysis due to high radioactivity of a matrix. Therefore it is necessary carrying out radiochemical separation of impurity radionuclides from matrix. Study of the literature datum have shown, that zirconium and niobium are very well extracted from muriatic solution with 5% tributyl phosphineoxide (TBPO) solution in toluene and 0,75 M solution of di-2-ethyl hexyl phosphoric acid (HDEHP) in cyclohexanone. Investigation of these elements extraction in these systems has shown that more effective and selective separation of matrix radionuclides is achieved in HDEHP-3M HCI system. This system is also extracted and hafnium, witch is an accompanying element of zirconium and its high content prevented determination of other impurity elements in sample. Therefore we used extraction system HDEHP-3M HCl for analysis of zirconium and zirconium-niobium alloys in chromatographic variant. By measurement of distribution profile of a matrix and of elution curve of determined elements is established, that for effective separation of impurity and matrix radionuclides there is enough chromatographic column with diameter 1 cm and height of a sorbent layer 7 cm, thus volume of elute, necessary for complete elution of determinate elements is 35-40 ml. On the basis of the carried out researches the technique of radiochemical NAA of high purity zirconium and zirconium-niobium alloy, which allows to

Method of reducing zirconium

International Nuclear Information System (INIS)

Megy, J.A.

1980-01-01

A method was developed for making nuclear-grade zirconium from a zirconium compound, which ismore economical than previous methods since it uses aluminum as the reductant metal rather than the more expensive magnesium. A fused salt phase containing the zirconium compound to be reduced is first prepared. The fused salt phase is then contacted with a molten metal phase which contains aluminum and zinc. The reduction is effected by mutual displacment. Aluminum is transported from the molten metal phase to the fused salt phase, replacing zirconium in the salt. Zirconium is transported from the fused salt phase to the molten metal phase. The fused salt phase and the molten metal phase are then separated, and the solvent metal and zirconium are separated by distillation or other means. (DN)

PLUTONIUM-ZIRCONIUM ALLOYS

Science.gov (United States)

Schonfeld, F.W.; Waber, J.T.

1960-08-30

A series of nuclear reactor fuel alloys consisting of from about 5 to about 50 at.% zirconium (or higher zirconium alloys such as Zircaloy), balance plutonium, and having the structural composition of a plutonium are described. Zirconium is a satisfactory diluent because it alloys readily with plutonium and has desirable nuclear properties. Additional advantages are corrosion resistance, excellent fabrication propenties, an isotropie structure, and initial softness.

ZIRCONIUM-CLADDING OF THORIUM

Science.gov (United States)

Beaver, R.J.

1961-11-21

A method of cladding thorium with zirconium is described. The quality of the bond achieved between thorium and zirconium by hot-rolling is improved by inserting and melting a thorium-zirconium alloy foil between the two materials prior to rolling. (AEC)

Metallurgy of zirconium and hafnium

International Nuclear Information System (INIS)

Baryshnikov, N.V.; Geger, V.Eh.; Denisova, N.D.; Kazajn, A.A.; Kozhemyakin, V.A.; Nekhamkin, L.G.; Rodyakin, V.V.; Tsylov, Yu.A.

1979-01-01

Considered are those properties of zirconium and of hafnium, which are of practical interest for the manufacture of these elements. Systematized are the theoretical and the practical data on the procedures for thermal decomposition of zirconia and for obtaining zirconium dioxide and hafnium dioxide by a thermal decomposition of compounds and on the hydrometallurgical methods for extracting zirconium and hafnium. Zirconium and hafnium fluorides and chlorides production procedures are described. Considered are the iodide and the electrolytic methods of refining zirconium and hafnium

XANES analysis of dried and calcined bones

International Nuclear Information System (INIS)

Rajendran, Jayapradhi; Gialanella, Stefano; Aswath, Pranesh B.

2013-01-01

The structure of dried and calcined bones from chicken, bovine, deer, pig, sheep and chamois was examined using X-ray Absorption Near Edge Structure (XANES) spectroscopy. The oxygen K-edge absorption edge indicates that the surface of dried bone has a larger proportion of carbonate than the interior that is made up of phosphates. The phosphorus L and K edge clearly indicate that pyrophosphates, α-tricalcium phosphate (α-TCP) and hydrogen phosphates of Ca do not exist in either the dried bone or calcined bone and phosphorus exists as either β-tricalcium phosphate (β-TCP) or hydroxyapatite, both in the dried and calcined conditions. The Ca K-edge analysis indicates that β-TCP is the likely form of phosphate in both the dried and calcined conditions. - Highlights: • For the first time bones of five different species of vertebrates have been compared in both the dried and calcined states. • O, P and Ca edges detail the local coordination of these atoms in dried and calcined bone. • O K-edge shows that the surface of bone has more CO 3 while the interior has more PO 4 . • P and Ca edges eliminate the presence of pyrophosphates and confirmed the presence of HA and β-TCP. • The stability of these phosphates on calcination has been examined using XANES

XANES analysis of dried and calcined bones

Energy Technology Data Exchange (ETDEWEB)

Rajendran, Jayapradhi [Materials Science and Engineering Department, University of Texas at Arlington (United States); Gialanella, Stefano [Materials Science and Industrial Technology Department, University of Trento (Italy); Aswath, Pranesh B., E-mail: aswath@uta.edu [Materials Science and Engineering Department, University of Texas at Arlington (United States)

2013-10-15

The structure of dried and calcined bones from chicken, bovine, deer, pig, sheep and chamois was examined using X-ray Absorption Near Edge Structure (XANES) spectroscopy. The oxygen K-edge absorption edge indicates that the surface of dried bone has a larger proportion of carbonate than the interior that is made up of phosphates. The phosphorus L and K edge clearly indicate that pyrophosphates, α-tricalcium phosphate (α-TCP) and hydrogen phosphates of Ca do not exist in either the dried bone or calcined bone and phosphorus exists as either β-tricalcium phosphate (β-TCP) or hydroxyapatite, both in the dried and calcined conditions. The Ca K-edge analysis indicates that β-TCP is the likely form of phosphate in both the dried and calcined conditions. - Highlights: • For the first time bones of five different species of vertebrates have been compared in both the dried and calcined states. • O, P and Ca edges detail the local coordination of these atoms in dried and calcined bone. • O K-edge shows that the surface of bone has more CO{sub 3} while the interior has more PO{sub 4}. • P and Ca edges eliminate the presence of pyrophosphates and confirmed the presence of HA and β-TCP. • The stability of these phosphates on calcination has been examined using XANES.

Synthesis of zirconium by zirconium tetrachloride reduction by magnesio-thermia. Experimental study and modelling; Elaboration de zirconium par reduction de tetrachlorure de zirconium par magnesothermie. Etude experimentale et modelisation

Energy Technology Data Exchange (ETDEWEB)

Basin, N

2001-01-01

This work deals with the synthesis of zirconium. The ore is carbo-chlorinated to obtain the tetrachloride which is then purified by selective condensation and extractive distillation. Zirconium tetrachloride is then reduced by magnesium and the pseudo-alloy is obtained according to the global following reaction (Kroll process): ZrCl{sub 4} + 2 Mg = 2 MgCl{sub 2}. By thermodynamics, it has been shown that the volatilization of magnesium chloride and the formation of zirconium sub-chlorides are minimized when the combined effects of temperature and of dilution with argon are limited. With these conditions, the products, essentially zirconium and magnesium chloride, are obtained in equivalence ratio in the magnesio-thermia reaction. The global kinetics of the reduction process has been studied by a thermal gravimetric method. A thermo-balance device has been developed specially for this kinetics study. It runs under a controlled atmosphere and is coupled to a vapor tetrachloride feed unit. The transformation is modelled supposing that the zirconium and magnesium chloride formation result: 1)of the evaporation of magnesium from its liquid phase 2)of the transfer of magnesium and zirconium tetrachloride vapors towards the front of the reaction located in the gaseous phase 3)of the chemical reaction. In the studied conditions, the diffusion is supposed to be the limiting process. The influence of the following parameters: geometry of the reactive zone, temperature, scanning rate of the argon-zirconium tetrachloride mixture, composition of the argon-zirconium tetrachloride mixture has been experimentally studied and confronted with success to the model. (O.M.)

Zirconium - an imported mineral commodity

International Nuclear Information System (INIS)

1983-10-01

This report examines Canada's position in regard to the principal zirconium materials: zircon; fusion-cast zirconium-bearing refractory products; zirconium-bearing chemicals; and zirconium metal, master alloys, and alloys. None of these is produced in Canada except fused alumina-zirconia and certain magnesium-zirconium alloys and zirconium-bearing steels. Most of the 3 000-4 000 tonnes of the various forms of zircon believed to be consumed in Canada each year is for foundry applications. Other minerals, notably chromite, olivine and silica sand are also used for these purposes and, if necessary, could be substituted for zircon. Zirconium's key role in Canada is in CANDU nuclear power reactors, where zirconium alloys are essential in the cladding for fuel bundles and in capital equipment such as pressure tubes, calandria tubes and reactivity control mechanisms. If zirconium alloys were to become unavailable, the Canadian nuclear power industry would collapse. As a contingency measure, Ontario Hydro maintains at least nine months' stocks of nuclear fuel bundles. Canada's vulnerability to short-term disruptions to supplies of nuclear fuel is diminished further by the availability of more expensive electricity from non-nuclear sources and, given time, from mothballed thermal plants. Zirconium minerals are present in many countries, notably Australia, the Republic of South Africa and the United States. Australia is Canada's principal source of zircon imports; South Africa is its sole source of baddeleyite. At this time, there are no shortages of either material. Canada has untapped zirconium resources in the Athabasca Oil Sands (zircon) and at Strange Lake along the ill-defined border between Quebec and Newfoundland (gittinsite). Adequate metal and alloy production facilities exist in France, Japan and the United States. No action by the federal government in regard to zirconium supplies is called for at this time

Process for purifying zirconium sponge

International Nuclear Information System (INIS)

Abodishish, H.A.M.; Kimball, L.S.

1992-01-01

This patent describes a Kroll reduction process wherein a zirconium sponge contaminated with unreacted magnesium and by-product magnesium chloride is produced as a regulus, a process for purifying the zirconium sponge. It comprises: distilling magnesium and magnesium chloride from: a regulus containing a zirconium sponge and magnesium and magnesium chloride at a temperature above about 800 degrees C and at an absolute pressure less than about 10 mmHg in a distillation vessel to purify the zirconium sponge; condensing the magnesium and the magnesium chloride distilled from the zirconium sponge in a condenser; and then backfilling the vessel containing the zirconium sponge and the condenser containing the magnesium and the magnesium chloride with a gas; recirculating the gas between the vessel and the condenser to cool the zirconium sponge from above about 800 degrees C to below about 300 degrees C; and cooling the recirculating gas in the condenser containing the condensed magnesium and the condensed magnesium chloride as the gas cools the zirconium sponge to below about 300 degrees C

Bin Set 1 Calcine Retrieval Feasibility Study

International Nuclear Information System (INIS)

Adams, R.D.; Berry, S.M.; Galloway, K.J.; Langenwalter, T.A.; Lopez, D.A.; Noakes, C.M.; Peterson, H.K.; Pope, M.I.; Turk, R.J.

1999-01-01

At the Department of Energy's Idaho Nuclear Technology and Engineering Center, as an interim waste management measure, both mixed high-level liquid waste and sodium bearing waste have been solidified by a calculation process and are stored in the Calcine Solids Storage Facilities. This calcined product will eventually be treated to allow final disposal in a national geologic repository. The Calcine Solids Storage Facilities comprise seven ''bit sets.'' Bin Set 1, the first to be constructed, was completed in 1959, and has been in service since 1963. It is the only bin set that does not meet current safe-shutdown earthquake seismic criteria. In addition, it is the only bin set that lacks built-in features to aid in calcine retrieval. One option to alleviate the seismic compliance issue is to transport the calcine from Bin Set 1 to another bin set which has the required capacity and which is seismically qualified. This report studies the feasibility of retrieving the calcine from Bi n Set 1 and transporting it into Bin Set 6 which is located approximately 650 feet away. Because Bin Set 1 was not designed for calcine retrieval, and because of the high radiation levels and potential contamination spread from the calcined material, this is a challenging engineering task. This report presents preconceptual design studies for remotely-operated, low-density, pneumatic vacuum retrieval and transport systems and equipment that are based on past work performed by the Raytheon Engineers and Constructors architectural engineering firm. The designs presented are considered feasible; however, future development work will be needed in several areas during the subsequent conceptual design phase

Bin Set 1 Calcine Retrieval Feasibility Study

Energy Technology Data Exchange (ETDEWEB)

R. D. Adams; S. M. Berry; K. J. Galloway; T. A. Langenwalter; D. A. Lopez; C. M. Noakes; H. K. Peterson; M. I. Pope; R. J. Turk

1999-10-01

At the Department of Energy's Idaho Nuclear Technology and Engineering Center, as an interim waste management measure, both mixed high-level liquid waste and sodium bearing waste have been solidified by a calculation process and are stored in the Calcine Solids Storage Facilities. This calcined product will eventually be treated to allow final disposal in a national geologic repository. The Calcine Solids Storage Facilities comprise seven ''bit sets.'' Bin Set 1, the first to be constructed, was completed in 1959, and has been in service since 1963. It is the only bin set that does not meet current safe-shutdown earthquake seismic criteria. In addition, it is the only bin set that lacks built-in features to aid in calcine retrieval. One option to alleviate the seismic compliance issue is to transport the calcine from Bin Set 1 to another bin set which has the required capacity and which is seismically qualified. This report studies the feasibility of retrieving the calcine from Bi n Set 1 and transporting it into Bin Set 6 which is located approximately 650 feet away. Because Bin Set 1 was not designed for calcine retrieval, and because of the high radiation levels and potential contamination spread from the calcined material, this is a challenging engineering task. This report presents preconceptual design studies for remotely-operated, low-density, pneumatic vacuum retrieval and transport systems and equipment that are based on past work performed by the Raytheon Engineers and Constructors architectural engineering firm. The designs presented are considered feasible; however, future development work will be needed in several areas during the subsequent conceptual design phase.

Contribution to the study of zirconium self-diffusion in zirconium carbide

International Nuclear Information System (INIS)

An, Chul

1972-01-01

The objective of this research thesis is to determine experimental conditions allowing the measurement of the self-diffusion coefficient of zirconium in zirconium carbide. The author reports the development of a method of preparation of zirconium carbide samples. He reports the use of ion implantation as technique to obtain a radio-tracer coating. The obtained results give evidence of the impossibility to use sintered samples with small grains because of the demonstrated importance of intergranular diffusion. The self-diffusion coefficient is obtained in the case of zirconium carbide with grains having a diameter of few millimetres. The presence of 95 Nb from the disintegration of 95 Zr indicates that these both metallic elements have very close diffusion coefficients at 2.600 C [fr

Calcination/dissolution testing for Hanford Site tank wastes

International Nuclear Information System (INIS)

Colby, S.A.; Delegard, C.H.; McLaughlin, D.F.; Danielson, M.J.

1994-07-01

Thermal treatment by calcination offers several benefits for the treatment of Hanford Site tank wastes, including the destruction of organics and ferrocyanides and an hydroxide fusion that permits the bulk of the mostly soluble nonradioactive constituents to be easily separated from the insoluble transuranic residue. Critical design parameters were tested, including: (1) calciner equipment design, (2) hydroxide fusion chemistry, and (3) equipment corrosion. A 2 gal/minute pilot plant processed a simulated Tank 101-SY waste and produced a free flowing 700 C molten calcine with an average calciner retention time of 20 minutes and >95% organic, nitrate, and nitrite destruction. Laboratory experiments using actual radioactive tank waste and the simulated waste pilot experiments indicate that 98 wt% of the calcine produced is soluble in water, leaving an insoluble transuranic fraction. All of the Hanford Site tank wastes can benefit from calcination/dissolution processing, contingent upon blending various tank waste types to ensure a target of 70 wt% sodium hydroxide/nitrate/nitrite fluxing agent. Finally, corrosion testing indicates that a jacketed nickel liner cooled to below 400 C would corrode <2 mil/year (0.05 mm/year) from molten calcine attack

1st International Conference on Calcined Clays for Sustainable Concrete

CERN Document Server

Favier, Aurélie

2015-01-01

This volume focuses on research and practical issues linked to Calcined Clays for Sustainable Concrete. The main subjects are geology of clays, hydration and performance of blended systems with calcined clays, alkali activated binders, economic and environmental impacts of the use of calcined clays in cement based materials. Topics addressed in this book include the influence of processing on reactivity of calcined clays, influence of clay mineralogy on reactivity, geology of clay deposits, Portland-calcined clay systems, hydration, durability, performance, Portland-calcined clay-limestone systems, hydration, durability, performance, calcined clay-alkali systems, life cycle analysis, economics and environmental impact of use of calcined clays in cement and concrete, and field applications. This book compiles the different contributions of the 1st International Conference on Calcined Clays for Sustainable Concrete, which took place in Lausanne, Switzerland, June, 23-25, 2015.The papers present the latest  res...

Nanostructured zirconium titanate fibers prepared by particulate sol–gel and cellulose templating techniques

Energy Technology Data Exchange (ETDEWEB)

Rouhani, P. [Helmerich Advanced Technology Research Center, School of Electrical and Computer Engineering, Oklahoma State University, OK 74106 (United States); Salahinejad, E. [Helmerich Advanced Technology Research Center, School of Material Science and Engineering, Oklahoma State University, OK 74106 (United States); Department of Materials Science and Engineering, School of Engineering, Shiraz University, Zand Blvd., 7134851154 Shiraz (Iran, Islamic Republic of); Kaul, R. [Department of Biochemistry and Microbiology, Center for Health Sciences, Oklahoma State University, OK 74107 (United States); Vashaee, D. [Helmerich Advanced Technology Research Center, School of Electrical and Computer Engineering, Oklahoma State University, OK 74106 (United States); Tayebi, L., E-mail: lobat.tayebi@okstate.edu [Helmerich Advanced Technology Research Center, School of Material Science and Engineering, Oklahoma State University, OK 74106 (United States); School of Chemical Engineering, Oklahoma State University, Stillwater, OK 74078 (United States)

2013-08-15

Highlights: •A method to produce zirconium titanate fibers was introduced. •The resultant structure and photocatalytic activity of the fiber were investigated. •The fiber exhibited higher photocatalytic characteristics, compared with the powders. -- Abstract: In this paper, a method for cost-effective production of nanostructured zirconium titanate (ZrTiO{sub 4}) fibers is introduced. In this method, ZrTiO{sub 4} fibers were synthesized by a sol–gel technique using cellulose fibers as the template. The resultant structures were studied by transmission electron microscopy, X-ray diffraction, scanning electron microscopy, and Brunauer–Emmett–Teller (BET) analyses. The photocatalytic activity of the fiber was compared to that of ZrTiO{sub 4} powders prepared by the same sol–gel method, in dark and under UVA and UVC radiations. According to the results, after calcination accompanied by the template removal, the ZrTiO{sub 4} fiber consists of uniformly-deposited, crystalline nanoparticles. This nanostructured fiber exhibited a higher surface area and a higher porosity compared with the ZrTiO{sub 4} powders, resulting in considerably higher photocatalytic characteristics, as confirmed by the experiment. The large surface area and the enhanced photocatalytic activity of the ZrTiO{sub 4} fibers also offer applications in sensors and bioactive films.

Artefacts in multimodal imaging of titanium, zirconium and binary titanium-zirconium alloy dental implants: an in vitro study.

Science.gov (United States)

Smeets, Ralf; Schöllchen, Maximilian; Gauer, Tobias; Aarabi, Ghazal; Assaf, Alexandre T; Rendenbach, Carsten; Beck-Broichsitter, Benedicta; Semmusch, Jan; Sedlacik, Jan; Heiland, Max; Fiehler, Jens; Siemonsen, Susanne

2017-02-01

To analyze and evaluate imaging artefacts induced by zirconium, titanium and titanium-zirconium alloy dental implants. Zirconium, titanium and titanium-zirconium alloy implants were embedded in gelatin and MRI, CT and CBCT were performed. Standard protocols were used for each modality. For MRI, line-distance profiles were plotted to quantify the accuracy of size determination. For CT and CBCT, six shells surrounding the implant were defined every 0.5 cm from the implant surface and histogram parameters were determined for each shell. While titanium and titanium-zirconium alloy induced extensive signal voids in MRI owing to strong susceptibility, zirconium implants were clearly definable with only minor distortion artefacts. For titanium and titanium-zirconium alloy, the MR signal was attenuated up to 14.1 mm from the implant. In CT, titanium and titanium-zirconium alloy resulted in less streak artefacts in comparison with zirconium. In CBCT, titanium-zirconium alloy induced more severe artefacts than zirconium and titanium. MRI allows for an excellent image contrast and limited artefacts in patients with zirconium implants. CT and CBCT examinations are less affected by artefacts from titanium and titanium-zirconium alloy implants compared with MRI. The knowledge about differences of artefacts through different implant materials and image modalities might help support clinical decisions for the choice of implant material or imaging device in the clinical setting.

Artefacts in multimodal imaging of titanium, zirconium and binary titanium–zirconium alloy dental implants: an in vitro study

Science.gov (United States)

Schöllchen, Maximilian; Aarabi, Ghazal; Assaf, Alexandre T; Rendenbach, Carsten; Beck-Broichsitter, Benedicta; Semmusch, Jan; Sedlacik, Jan; Heiland, Max; Fiehler, Jens; Siemonsen, Susanne

2017-01-01

Objectives: To analyze and evaluate imaging artefacts induced by zirconium, titanium and titanium–zirconium alloy dental implants. Methods: Zirconium, titanium and titanium–zirconium alloy implants were embedded in gelatin and MRI, CT and CBCT were performed. Standard protocols were used for each modality. For MRI, line–distance profiles were plotted to quantify the accuracy of size determination. For CT and CBCT, six shells surrounding the implant were defined every 0.5 cm from the implant surface and histogram parameters were determined for each shell. Results: While titanium and titanium–zirconium alloy induced extensive signal voids in MRI owing to strong susceptibility, zirconium implants were clearly definable with only minor distortion artefacts. For titanium and titanium–zirconium alloy, the MR signal was attenuated up to 14.1 mm from the implant. In CT, titanium and titanium–zirconium alloy resulted in less streak artefacts in comparison with zirconium. In CBCT, titanium–zirconium alloy induced more severe artefacts than zirconium and titanium. Conclusions: MRI allows for an excellent image contrast and limited artefacts in patients with zirconium implants. CT and CBCT examinations are less affected by artefacts from titanium and titanium–zirconium alloy implants compared with MRI. The knowledge about differences of artefacts through different implant materials and image modalities might help support clinical decisions for the choice of implant material or imaging device in the clinical setting. PMID:27910719

Method of separating hafnium from zirconium

International Nuclear Information System (INIS)

Megy, J.A.

1980-01-01

English. A new anhydrous method was developed for separating zirconium and hafnium, which gives higher separation factors and is more economical than previous methods. A molten phase, comprising a solution of unseparated zirconium and hafnium and a solvent metal, is first prepared. The molten metal phase is contacted with a fused salt phase which includes a zirconium salt. Zirconium and hafnium separation is effected by mutual displacement with hafnium being transported from the molten metal phase to the fused salt phase, while zirconium is transported from the fused salt phase to the molten metal phase. The solvent metal is less electropositive than zirconium. Zinc was chosen as the solvent metal, from a group which also included cadmium, lead, bismuth, copper, and tin. The fused salt phase cations are more electropositive than zirconium and were selected from a group comprising the alkali elements, the alkaline earth elements, the rare earth elements, and aluminum. A portion of the zirconium in the molten metal phase was oxidized by injecting an oxidizing agent, chlorine, to form zirconium tetrachlorid

Effect of Bi on the corrosion resistance of zirconium alloys

International Nuclear Information System (INIS)

Yao Meiyi; Zhou Bangxin; Li Qiang; Zhang Weipeng; Zhu Li; Zou Linghong; Zhang Jinlong; Peng Jianchao

2014-01-01

In order to investigate systematically the effect of Bi addition on the corrosion resistance of zirconium alloys, different zirconium-based alloys, including Zr-4 (Zr-l.5Sn-0.2Fe-0.1Cr), S5 (Zr-0.8Sn-0.35Nb-0.4Fe-0.1Cr), T5 (Zr-0.7Sn-l.0Nb-0.3Fe-0.1Cr) and Zr-1Nb, were adopted to prepare the zirconium alloys containing Bi of 0∼0.5% in mass fraction. These alloys were denoted as Zr-4 + xBi, S5 + xBi, T5 + xBi and Zr-1Nb + xBi, respectively. The corrosion behavior of these specimens was investigated by autoclave testing in lithiated water with 0.01 M LiOH or deionized water at 360 ℃/18.6 MPa and in superheated steam at 400 ℃/10.3 MPa. The microstructure of the alloys was examined by TEM and the second phase particles (SPPs) were analyzed by EDS. Microstructure observation shows that the addition of Bi promotes the precipitation of Sn as second phase particles (SPPs) because Sn is in solid solution in α-Zr matrix in Zr-4, S5 and T5 alloys. The concentration of Bi dissolved in α-Zr matrix increase with the increase of Nb in the alloys, and the excess Bi precipitates as Bi-containing SPPs. The corrosion results show that the effect of Bi addition on the corrosion behavior of different zirconium-based alloys is very complicated, depending on their compositions and corrosion conditions. In the case of higher Bi concentration in α-Zr, the zirconium alloys exhibit better corrosion resistance. However, in the case of precipitation of Bi-containing SPPs, the corrosion resistance gets worse. This indicates that the solid solution of Bi in α-Zr matrix can improve the corrosion resistance, while the precipitation of the Bi-containing SPPs is harmful to the corrosion resistance. (authors)

Uranium dioxide calcining apparatus and method

International Nuclear Information System (INIS)

Cole, E.A.; Peterson, R.S.

1978-01-01

This invention relates to an improved continuous calcining apparatus for consistently and controllably producing from calcinable reactive solid compounds of uranium, such as ammonium diuranate, uranium dioxide (UO 2 ) having an oxygen to uranium ratio of less than 2.2. The apparatus comprises means at the outlet end of a calciner kiln for receiving hot UO 2 , means for cooling the UO 2 to a temperature of below 100 0 C and conveying the cooled UO 2 to storage or to subsequent UO 2 processing apparatus where it finally comes into contact with air, the means for receiving, cooling and conveying being sealed to the outlet end of the calciner and being maintained full of UO 2 and so operable as to exclude atmospheric oxygen from coming into contact with any UO 2 which is at elevated temperatures where it would readily oxidize, without the use of extra hydrogen gas in said means

Effect of additions of cerium, lanthanum, and zirconium on the state of plantinum and the activity of aluminoplatinum catalysts for the complete oxidation of hydrocarbons

International Nuclear Information System (INIS)

Drozdov, V.A.; Davydov, A.A.; Popovskii, V.V.; Tsyrul'nikov, P.G.

1986-01-01

It is shown from an analysis of the diffuse reflectance spectra that additions of cerium, lanthanum or zirconium to aluminoplatinum catalyst stabilize the platinum in an oxidized state. This leads to a change in the specific catalytic activity (SCA) towards the total oxidation of methane and butane. The SCA of modified, reduced samples is greater than the SCA of samples that were calcined in air. This is because of the greater activity of metallic platinum compared to the ionic form

Zirconium-barrier cladding attributes

International Nuclear Information System (INIS)

Rosenbaum, H.S.; Rand, R.A.; Tucker, R.P.; Cheng, B.; Adamson, R.B.; Davies, J.H.; Armijo, J.S.; Wisner, S.B.

1987-01-01

This metallurgical study of Zr-barrier fuel cladding evaluates the importance of three salient attributes: (1) metallurgical bond between the zirconium liner and the Zircaloy substrate, (2) liner thickness (roughly 10% of the total cladding wall), and (3) softness (purity). The effect that each of these attributes has on the pellet-cladding interaction (PCI) resistance of the Zr-barrier fuel was studied by a combination of analytical model calculations and laboratory experiments using an expanding mandrel technique. Each of the attributes is shown to contribute to PCI resistance. The effect of the zirconium liner on fuel behavior during off-normal events in which steam comes in contact with the zirconium surface was studied experimentally. Simulations of loss-of-coolant accident (LOCA) showed that the behavior of Zr-barrier cladding is virtually indistinguishable from that of conventional Zircaloy cladding. If steam contacts the zirconium liner surface through a cladding perforation and the fuel rod is operated under normal power conditions, the zirconium liner is oxidized more rapidly than is Zircaloy, but the oxidation rate returns to the rate of Zircaloy oxidation when the oxide phase reaches the zirconium-Zircaloy metallurgical bond

Calcination of the cerium concentrate to be cerium oxide

International Nuclear Information System (INIS)

Suyanti; MV Purwani

2016-01-01

Calcination of the cerium concentrate to be cerium oxide has done. The cerium concentrate were obtained from the Ce making process wear KBrO_3 and without using KBrO_3. The calcination were done with a variation of time 1, 2, 3 and 4 hours with the temperature variations of 700, 800 and 900°C. The easiest calcination of Ce concentrates to be CeO_2 containing majority of Ce(OH)_4 and contains least impurities as Th(OH)_4, (NH_4)_2Y(NO_3), H_4N_5O_1_2La, H_1_2N_3NdO_1_5 and N_3O_9Sm. On the calcination of Ce concentrates process results without using KBrO_3 1, the calcination temperature 900°C was obtained CeO_2 content of 73.53% for calcination time of 4 hours, has little difference when compared with the predictions and calculation result of complete calcination was equal 73.84%. (author)

Calcination under negative atmosphere for SYNROC preparation

International Nuclear Information System (INIS)

Ambashta, R.D.; Wattal, P.K.; Govindankutty, K.V.

2006-01-01

SYNROC-C is a ceramic waste formulation designed to immobilise reprocessing waste from fast breeder reactor. This formulation is capable of incorporating noble metals, other fission products, corrosion products and activation products in its multiphase assemblage. Calcination is an important step of SYNROC preparation for decomposition of nitrates of the radioactive waste and conversion to oxide precursors. This paper presents a comparison between properties of calcine prepared under different calcination procedures to obtain product suitable for compaction

Calcined Waste Storage at the Idaho Nuclear Technology and Engineering Center

Energy Technology Data Exchange (ETDEWEB)

Staiger, M. Daniel, Swenson, Michael C.

2011-09-01

This comprehensive report provides definitive volume, mass, and composition (chemical and radioactivity) of calcined waste stored at the Idaho Nuclear Technology and Engineering Center. Calcine composition data are required for regulatory compliance (such as permitting and waste disposal), future treatment of the caline, and shipping the calcine to an off-Site-facility (such as a geologic repository). This report also contains a description of the calcine storage bins. The Calcined Solids Storage Facilities (CSSFs) were designed by different architectural engineering firms and built at different times. Each CSSF has a unique design, reflecting varying design criteria and lessons learned from historical CSSF operation. The varying CSSF design will affect future calcine retrieval processes and equipment. Revision 4 of this report presents refinements and enhancements of calculations concerning the composition, volume, mass, chemical content, and radioactivity of calcined waste produced and stored within the CSSFs. The historical calcine samples are insufficient in number and scope of analysis to fully characterize the entire inventory of calcine in the CSSFs. Sample data exist for all the liquid wastes that were calcined. This report provides calcine composition data based on liquid waste sample analyses, volume of liquid waste calcined, calciner operating data, and CSSF operating data using several large Microsoft Excel (Microsoft 2003) databases and spreadsheets that are collectively called the Historical Processing Model. The calcine composition determined by this method compares favorably with historical calcine sample data.

Calcined Waste Storage at the Idaho Nuclear Technology and Engineering Center

International Nuclear Information System (INIS)

Staiger, M. Daniel; Swenson, Michael C.

2011-01-01

This comprehensive report provides definitive volume, mass, and composition (chemical and radioactivity) of calcined waste stored at the Idaho Nuclear Technology and Engineering Center. Calcine composition data are required for regulatory compliance (such as permitting and waste disposal), future treatment of the caline, and shipping the calcine to an off-Site-facility (such as a geologic repository). This report also contains a description of the calcine storage bins. The Calcined Solids Storage Facilities (CSSFs) were designed by different architectural engineering firms and built at different times. Each CSSF has a unique design, reflecting varying design criteria and lessons learned from historical CSSF operation. The varying CSSF design will affect future calcine retrieval processes and equipment. Revision 4 of this report presents refinements and enhancements of calculations concerning the composition, volume, mass, chemical content, and radioactivity of calcined waste produced and stored within the CSSFs. The historical calcine samples are insufficient in number and scope of analysis to fully characterize the entire inventory of calcine in the CSSFs. Sample data exist for all the liquid wastes that were calcined. This report provides calcine composition data based on liquid waste sample analyses, volume of liquid waste calcined, calciner operating data, and CSSF operating data using several large Microsoft Excel (Microsoft 2003) databases and spreadsheets that are collectively called the Historical Processing Model. The calcine composition determined by this method compares favorably with historical calcine sample data.

Localized deformation of zirconium-liner tube

International Nuclear Information System (INIS)

Nagase, Fumihisa; Uchida, Masaaki

1988-03-01

Zirconium-liner tube has come to be used in BWR. Zirconium liner mitigates the localized stress produced by the pellet-cladding interaction (PCI). In this study, simulating the ridging, stresses were applied to the inner surfaces of zirconium-liner tubes and Zircaloy-2 tubes, and, to investigate the mechanism and the extent of the effect, the behavior of zirconium liner was examined. As the result of examination, stress was concentrated especially at the edge of the deformed region, where zirconium liner was highly deformed. Even after high stress was applied, the deformation of Zircaloy part was small, since almost the concentrated stress was mitigated by the deformation of zirconium liner. In addition, stress and strain distributions in the cross section of specimen were calculated with a computer code FEMAXI-III. The results also showed that zirconium liner mitigated the localized stress in Zircaloy, although the affected zone was restricted to the region near the boundary between zirconium liner and Zircaloy. (author)

A simple dissolved metals mixing method to produce high-purity MgTiO3 nanocrystals

International Nuclear Information System (INIS)

Pratapa, Suminar; Baqiya, Malik A.; Istianah,; Lestari, Rina; Angela, Riyan

2014-01-01

A simple dissolved metals mixing method has been effectively used to produce high-purity MgTiO 3 (MT) nanocrystals. The method involves the mixing of independently dissolved magnesium and titanium metal powders in hydrochloric acid followed by calcination. The phase purity and nanocrystallinity were determined by making use of laboratory x-ray diffraction data, to which Rietveld-based analyses were performed. Results showed that the method yielded only one type magnesium titanate powders, i.e. MgTiO 3 , with no Mg 2 TiO 4 or MgTi 2 O 5 phases. The presence of residual rutile or periclase was controlled by adding excessive Mg up to 5% (mol) in the stoichiometric mixing. The method also resulted in MT nanocrystals with estimated average crystallite size of 76±2 nm after calcination at 600°C and 150±4 nm (at 800°C). A transmission electron micrograph confirmed the formation of the nanocrystallites

Zirconium isotope separation process

International Nuclear Information System (INIS)

Peterson, S.H.; Lahoda, E.J.

1988-01-01

A process is described for reducing the amount of zirconium 91 isotope in zirconium comprising: forming a first solution of (a) a first solvent, (b) a scavenger, and (c) a zirconium compound which is soluble in the first solvent and reacts with the scavenger when exposed to light of a wavelength of 220 to 600 nm; irradiating the first solution with light at the wavelength for a time sufficient to photoreact a disproportionate amount of the zirconium compound containing the zirconium 91 isotope with the scavenger to form a reaction product in the first solution; contacting the first solution, while effecting the irradiation, with a second solvent which is immiscible with the first solvent, which the second solvent is a preferential solvent for the reaction product relative to the first solvent, such that at least a portion of the reaction product is transferred to the second solvent to form a second solution; and separating the second solution from the first solution after the contacting

Zirconium for nitric acid solutions

International Nuclear Information System (INIS)

Yau, T.L.

1984-01-01

The excellent corrosion resistance of zirconium in nitric acid has been known for over 30 years. Recently, there is an increasing interest in using zirconium for nitric acid services. Therefore, an extensive research effort has been carried out to achieve a better understanding of the corrosion properties of zirconium in nitric acid. Particular attention is paid to the effect of concentration, temperature, structure, solution impurities, and stress. Immersion, autoclave, U-bend, and constant strain-rate tests were used in this study. Results of this study indicate that the corrosion resistance of zirconium in nitric acid is little affected by changes in temperature and concentration, and the presence of common impurities such as seawater, sodium chloride, ferric chloride, iron, and stainless steel. Moreover, the presence of seawater, sodium chloride, ferric chloride, and stainless steel has little effect on the stress corrosion craking (SCC) susceptibility of zirconium in 70% nitric acid at room temperatures. However, zirconium could be attacked by fluoride-containing nitric acid and the vapors of chloride-containing nitric acid. Also, high sustained tensile stresses should be avoided when zirconium is used to handle 70% nitric acid at elevated temperatures or > 70% nitric acid

Activity and structure of calcined coal gangue

Energy Technology Data Exchange (ETDEWEB)

Gong Chenchen; Li Dongxu; Wang Xiaojun; Li Zongjin [Nanjing University of Technology, Nanjing (China). College of Materials Science and Engineering

2007-12-15

Coal gangue was activated by means of calcination in seven temperature ranges. Systematic research was made about activation mechanism and structural evolution. The glycerin-ethanol method, SEM, MIP and XRD were used to determine the variation of structure and activation of coal gangue during calcination. The experimental results show that because of heat treatment in the range of calcination temperatures, mineral composition and microstructure of coal gangue are changed. In addition, its activity is improved. The amount of lime absorbed by the sample calcined at 700{sup o}C is 2-4 times that by uncalcined coal gangue in the course of hydration. When NaOH is added to coal gangue-lime system, the hydration reaction rate of the system is increased and the microstructure of hydrating samples of coal gangue is improved.

Experimental and thermodynamic study of the erbium-oxygen-zirconium and gadolinium-oxygen-zirconium systems

International Nuclear Information System (INIS)

Jourdan, J.

2009-11-01

This work is a contribution to the development of innovative concepts for fuel cladding in pressurized water nuclear reactors. This concept implies the insertion of rare earth (erbium and gadolinium) in the zirconium fuel cladding. The determination of phase equilibria in the systems is essential prior to the implementation of such a promising solution. This study consisted in an experimental determination of the erbium-zirconium phase diagram. For this, we used many different techniques in order to obtain diagram data such as solubility limits, solidus, liquidus or invariant temperatures. These data allowed us to present a new diagram, very different from the previous one available in the literature. We also assessed the diagram using the CALPHAD approach. In the gadolinium-zirconium system, we determined experimentally the solubility limits. Those limits had never been determined before, and the values we obtained showed a very good agreement with the experimental and assessed versions of the diagram. Because these alloys are subjected to oxygen diffusion throughout their life, we focused our attention on the erbium-oxygen-zirconium and gadolinium-oxygen-zirconium systems. The first system has been investigated experimentally. The alloys fabrication has been performed using powder metallurgy. In order to obtain pure raw materials, we fabricated powder from erbium and zirconium bulk metals using hydrogen absorption/desorption. The characterisation of the ternary pellets allowed the determination of two ternary isothermal sections at 800 and 1100 C. For the gadolinium-oxygen-zirconium system, we calculated the phase equilibria at temperatures ranging from 800 to 1100 C, using a homemade database compiled from literature assessments of the oxygen-zirconium, gadolinium-zirconium and gadolinia-zirconia systems. Finally, we determined the mechanical properties, in connexion with the microstructure, of industrial quality alloys in order to identify the influence of

Zirconium and cast zirconium

Energy Technology Data Exchange (ETDEWEB)

Krone, K

1977-04-01

A survey is given on the occurence of zirconium, production of Zr sponge and semi-finished products, on physical and mechanical properties, production of Zr cast, composition of the commercial grades and reactor grades qualities, metal cutting, welding, corrosion behavior and use.

Synthesis of zirconium by zirconium tetrachloride reduction by magnesio-thermia. Experimental study and modelling

International Nuclear Information System (INIS)

Basin, N.

2001-01-01

This work deals with the synthesis of zirconium. The ore is carbo-chlorinated to obtain the tetrachloride which is then purified by selective condensation and extractive distillation. Zirconium tetrachloride is then reduced by magnesium and the pseudo-alloy is obtained according to the global following reaction (Kroll process): ZrCl 4 + 2 Mg = 2 MgCl 2 . By thermodynamics, it has been shown that the volatilization of magnesium chloride and the formation of zirconium sub-chlorides are minimized when the combined effects of temperature and of dilution with argon are limited. With these conditions, the products, essentially zirconium and magnesium chloride, are obtained in equivalence ratio in the magnesio-thermia reaction. The global kinetics of the reduction process has been studied by a thermal gravimetric method. A thermo-balance device has been developed specially for this kinetics study. It runs under a controlled atmosphere and is coupled to a vapor tetrachloride feed unit. The transformation is modelled supposing that the zirconium and magnesium chloride formation result: 1)of the evaporation of magnesium from its liquid phase 2)of the transfer of magnesium and zirconium tetrachloride vapors towards the front of the reaction located in the gaseous phase 3)of the chemical reaction. In the studied conditions, the diffusion is supposed to be the limiting process. The influence of the following parameters: geometry of the reactive zone, temperature, scanning rate of the argon-zirconium tetrachloride mixture, composition of the argon-zirconium tetrachloride mixture has been experimentally studied and confronted with success to the model. (O.M.)

Fluidized-bed calcination of simulated commercial high-level radioactive wastes

International Nuclear Information System (INIS)

Freeby, W.A.

1975-11-01

Work is in progress at the Idaho Chemical Processing Plant to verify process flowsheets for converting simulated commercial high-level liquid wastes to granular solids using the fluidized-bed calcination process. Primary emphasis in the series of runs reported was to define flowsheets for calcining simulated Allied-General Nuclear Services (AGNS) waste and to evaluate product properties significant to calcination, solids storage, or post treatment. Pilot-plant studies using simulated high-level acid wastes representative of those to be produced by Nuclear Fuel Services, Inc. (NFS) are also included. Combined AGNS high-level and intermediate-level waste (0.26 M Na in blend) was successfully calcined when powdered iron was added (to result in a Na/Fe mole ratio of 1.0) to the feed to prevent particle agglomeration due to sodium nitrate. Long-term runs (approximately 100 hours) showed that calcination of the combined waste is practical. Concentrated AGNS waste containing sodium at concentrations less than 0.2 M were calcined successfully; concentrated waste containing 1.13 M Na calcined successfully when powdered iron was added to the feed to suppress sodium nitrate formation. Calcination of dilute AGNS waste by conventional fluid-bed techniques was unsuccessful due to the inability to control bed particle size--both particle size and bed level decreased. Fluid-bed solidification of AGNS dilute waste at conditions in which most of the calcined solids left the calciner vessel with the off-gas was successful. In such a concept, the steady-state composition of the bed material would be approximately 22 wt percent calcined solids deposited on inert particles. Calcination of simulated NFS acid waste indicated that solidification by the fluid-bed process is feasible

Calcine Waste Storage at the Idaho Nuclear Technology and Engineering Center

Energy Technology Data Exchange (ETDEWEB)

M. D. Staiger

1999-06-01

A potential option in the program for long-term management of high-level wastes at the Idaho Nuclear Technology and Engineering Center (INTEC), at the Idaho National Engineering and Environmental Laboratory, calls for retrieving calcine waste and converting it to a more stable and less dispersible form. An inventory of calcine produced during the period December 1963 to May 1999 has been prepared based on calciner run, solids storage facilities operating, and miscellaneous operational information, which gives the range of chemical compositions of calcine waste stored at INTEC. Information researched includes calciner startup data, waste solution analyses and volumes calcined, calciner operating schedules, solids storage bin capacities, calcine storage bin distributor systems, and solids storage bin design and temperature monitoring records. Unique information on calcine solids storage facilities design of potential interest to remote retrieval operators is given.

Retrieval System for Calcined Waste for the Idaho Cleanup Project - 12104

Energy Technology Data Exchange (ETDEWEB)

Eastman, Randy L.; Johnston, Beau A.; Lower, Danielle E. [CH2M-WG Idaho, LLC. The Idaho Cleanup Project at the Idaho National Laboratory (United States)

2012-07-01

This paper describes the conceptual approach to retrieve radioactive calcine waste, hereafter called calcine, from stainless steel storage bins contained within concrete vaults. The retrieval system will allow evacuation of the granular solids (calcine) from the storage bins through the use of stationary vacuum nozzles. The nozzles will use air jets for calcine fluidization and will be able to rotate and direct the fluidization or displacement of the calcine within the bin. Each bin will have a single retrieval system installed prior to operation to prevent worker exposure to the high radiation fields. The addition of an articulated camera arm will allow for operations monitoring and will be equipped with contingency tools to aid in calcine removal. Possible challenges (calcine bridging and rat-holing) associated with calcine retrieval and transport, including potential solutions for bin pressurization, calcine fluidization and waste confinement, are also addressed. The Calcine Disposition Project has the responsibility to retrieve, treat, and package HLW calcine. The calcine retrieval system has been designed to incorporate the functions and technical characteristics as established by the retrieval system functional analysis. By adequately implementing the highest ranking technical characteristics into the design of the retrieval system, the system will be able to satisfy the functional requirements. The retrieval system conceptual design provides the means for removing bulk calcine from the bins of the CSSF vaults. Top-down vacuum retrieval coupled with an articulating camera arm will allow for a robust, contained process capable of evacuating bulk calcine from bins and transporting it to the processing facility. The system is designed to fluidize, vacuum, transport and direct the calcine from its current location to the CSSF roof-top transport lines. An articulating camera arm, deployed through an adjacent access riser, will work in conjunction with the

Neutron activation of chlorine in zirconium and zirconium alloys use of the matrix as comparator

International Nuclear Information System (INIS)

Cohen, I.M.; Gomez, C.D.; Mila, M.I.

1981-01-01

A procedure is described for neutron activation analysis of chlorine in zirconium and zirconium alloys. Calculation of chlorine concentration is performed relative to zirconium concentration in the matrix in order to minimize effects of differences in irradiation and counting geometry. Principles of the method and the results obtained are discussed. (author)

Development and evaluation of alumina calcination

International Nuclear Information System (INIS)

Bennett, I.J.

2000-01-01

This thesis focuses on a number of aspects governing the transformation of gibbsite, via intermediate phases, to α-alumina. These aspects include the size and morphology of the gibbsite grains, the influence of additions of foreign elements, the effect of a mechanical treatment of the gibbsite prior to calcination, and combinations of these factors. The materials were characterised by scanning electron microscopy, X-ray diffraction and surface area measurements. For some of the calcined materials an attempt was made to sinter the powders to a dense body to investigate if any of the treatments during calcination had an effect on this process. The literature review covers the current state of understanding of the production of bulk alumina powder by the Bayer process and the phase changes seen on calcination of precursors to the stable α-alumina phase. A detailed description of the phase changes is given and the various routes and conditions necessary for the transformations to occur are considered. The transformations are examined in relation to the morphology of the crystals and the variables controlling the phase transformation route are discussed. Calcination in air showed that the size of the gibbsite grain governs the calcination route taken to reach oc-alumina. The standard gibbsites used in this work show a mixed calcination sequence transforming both via the boehmite phase, followed by the γ, δ and θ phases, and via the χ and κ phases. The formation of boehmite is attributed to retention of water vapour within the grain. Differences in morphology of the starting materials showed that for the range of materials seen, the morphology of the grain is less important than its size. The super fine material confirmed that a small grain size transforms via the non-boehmite route only, with the other gibbsites taking intermediate routes as for the standard gibbsites. Of the additions made prior to calcination, aluminium fluoride was found to reduce the

Microwave heating application in calcination and SYNROC formation

International Nuclear Information System (INIS)

Ambashta, R.D.; Wattal, P.K.; Malav, R.K.; Mallik, G.K.

2006-01-01

Microwave for calcination of titanate based ceramic wasteform (SYNROC) is being reported for the first time in this paper. Although major constituents in SYNROC were non microwave active, the combination with microwave active constituents rendered the mixture calcinable. Calcine was sintered at 1150 degC under hot uniaxial conditions at an applied pressure of ∼30 MPa. XRD shows presence of major phases of SYNROC in the compacted sample. (author)

Fixation of calcined waste by bituminization or cementation

International Nuclear Information System (INIS)

Napravnik, J.; Kyrs, M.; Ditl, P.

1983-01-01

The overall concept is given of the combination of calcination with fixation into bitumen, cement etc. The design is shown of a calciner with the capacity of 10 L/h which was tested on real radioactive wastes for 2000 h. The geometrical and operating parameters of the apparatus have been optimized based on a statistical evaluation of the experiments. Wastes containing nitrates are calcined at 300-550 deg. C, yielding oxides. Wastes containing sulphates, carbonates, KMnO 4 , or borates are calcined at 150-330 deg. C, yielding soluble salts. The content of H 3 BO 4 and Na 2 B 4 O 7 and in some cases of sulphates in the calcinate retards hardening of the mixture with cement. Nitrates and detergents also interfere. The effect of the above components on the products mixed with bitumen is much less. Detergents can be decomposed at 200-300 deg. C; organic acids can be reacted with A1 salts to form insoluble substances lowering the leaching rate of Sr and Cs; small amounts of SiO 2 eliminate the effect of borates on cement hardening. The drawbacks of bituminization with bitumen emulsions are the complicated preparation of the emulsion, higher leaching rate of the product and low stability of the emulsion against breaking. The leachability was determined (1-50 days) of different products containing LWR wastes: 33% of concentrated waste in cement of calcination product stabilized with PVA exhibit approx. 8x10 - 3 g/cm 2 per day, 33% of calcine in cement approx. 3x10 - 3 ; 40% concentrate fixed with bitumen emulsion approx. 9x10 - 4 ; 50% calcine stabilized with PVA in bitumen, pilot-plant scale approx. 2x10 - 5 ; the same but on a laboratory scale approx. 1.10 - 5 . (author)

Mathematical modeling of an in-line low-NOx calciner

DEFF Research Database (Denmark)

Iliuta, Ion; Dam-Johansen, Kim; Jensen, Lars Skaarup

2002-01-01

The reduction of the NOx content in in-line-calciner-type kiln systems can be made by optimization of the primary filing in the rotary kiln and of the secondary firing in the calciner. Because the optimization of calciner offers greater opportunities the mathematical modeling of this reactor...

Product removal and solids transport from fluidized-bed calciners

International Nuclear Information System (INIS)

Grimmett, E.S.; Munger, D.H.

1978-09-01

Methods of removing the solid product from pilot-plant and production fluidized-bed calciners, and transporting product to underground storage vaults are reported here. Testing of dense-phase solids transport systems in test loops during development of a 15-cm-diam. and 30-cm-diam. calciner are described. A lean-phase solid transport system is used with the Waste Calcining Facility. The results of some recent tests done in a lean-phase transport system connected to the 30-cm-diam. calciner are included in this report

Extraction of zirconium from raffinate stream of Zirconium Oxide Plant raffinate

International Nuclear Information System (INIS)

Pandey, Garima; Chinchale, R.; Renjith, A.U.; Mukhopadhyay, S.; Shenoy, K.T.; Ghosh, S.K.

2013-01-01

Recovery of metals from dilute streams is a major task in nuclear industry in the view of environmental remediation and value recovery. Presently solvent extraction process is employed on the commercial scale to recover nuclear pure zirconium using TBP as extractant. The waste stream of TBP extraction process contains about 1.2 gpl of Zirconium in nitrate form. At present there is no process to recover Zirconium from this raffinate stream. Hence, under the present study recovery of zirconium from the raffinate stream of Zirconium Oxide Plant Raffinate has been investigated. TBP, which is the most commonly used solvent in the nuclear industry is not suitable for the extraction of zirconium from lean solution at low acidity as its distribution coefficient is less than one. In search of a suitable extractant Mixed Alkyl Phosphine Oxide (MAPO) was investigated as potential carrier. Parametric batch studies for various equilibrium data like extractant concentration, strippant concentration, solvent reusability, equilibration time, acidity etc. were done to optimize the process condition. For the distribution studies, equal volumes of the raffinate and organic phase were shaken at room temperature in digital wrist action shaker for 10 minutes to ensure complete equilibrium. It was found that 0.1 M MAPO in 80:20 dodecane: isodecanol is suitable for extraction of Zr at 2 N acidity. 0.1 M MAPO gives distribution coefficient in the range of 12-15 for Zr. The slope of log-log plot between MAPO concentration and K, suggests involvement of 3 molecules of MAPO in the formation of extracting species. 0.2 M Oxalic acid was able to completely back extract Zr from the organic phase into aqueous phase. Also good regeneration capacity of MAPO projects its potential to be used as extractant for the process. Based on the equilibrium studies, Dispersion Liquid Membrane configuration in hollow fiber contactor was explored for the extraction of Zirconium from Zirconium Nitrate Pure

Determination of hydrogen in zirconium hydride and uranium-zirconium hydride by inert gas exraction-gravimetric method

International Nuclear Information System (INIS)

Hoshino, Akira; Iso, Shuichi

1976-01-01

An inert gas extraction-gravimetric method has been applied to the determination of hydrogen in zirconium hydride and uranium-zirconium hydride which are used as neutron moderator and fuel of nuclear safety research reactor (NSRR), respectively. The sample in a graphite-enclosed quartz crucible is heated inductively to 1200 0 C for 20 min in a helium stream. Hydrogen liberated from the sample is oxidized to water by copper(I) oxide-copper(II) oxide at 400 0 C, and the water is determined gravimetrically by absorption in anhydrone. The extraction curves of hydrogen for zirconium hydride and uranium-zirconium hydride samples are shown in Figs. 2 and 3. Hydrogen in the samples is extracted quantitatively by heating at (1000 -- 1250) 0 C for (10 -- 40) min. Recoveries of hydrogen in the case of zirconium hydride were examined as follows: a weighed zirconium rod (5 phi x 6 mm, hydrogen -5 Torr. After the chamber was filled with purified hydrogen to 200 Torr, the rod was heated to 400 0 C for 15 h, and again weighed to determine the increase in weight. Hydrogen in the rod was then determined by the proposed method. The results are in excellent agreement with the increase in weight as shown in Table 1. Analytical results of hydrogen in zirconium hydride samples and an uranium-zirconium hydride sample are shown in Table 2. (auth.)

Modification in band gap of zirconium complexes

Energy Technology Data Exchange (ETDEWEB)

Sharma, Mayank, E-mail: mayank30134@gmail.com; Singh, J.; Chouhan, S. [Department of Physics, ISLE, IPS Academy, Indore (M.P.) (India); Mishra, A. [School of Physics, Devi Ahilya Vishwavidyalaya, Indore (M.P.) (India); Shrivastava, B. D. [Govt. P. G. College, Biora (M.P.) (India)

2016-05-06

The optical properties of zirconium complexes with amino acid based Schiff bases are reported here. The zirconium complexes show interesting stereo chemical features, which are applicable in organometallic and organic synthesis as well as in catalysis. The band gaps of both Schiff bases and zirconium complexes were obtained by UV-Visible spectroscopy. It was found that the band gap of zirconium complexes has been modified after adding zirconium compound to the Schiff bases.

Design and development of a rotary calciner for radiochemical waste

International Nuclear Information System (INIS)

Pande, D.P.; Sutar, V.D.; Sengar, P.B.S.

1997-01-01

Present experience and knowledge in handling of radioactive waste has led to identification of major thrust areas in the development of the treatment processes. In order to reduce evaporation and volatility losses in the vitrification facility, it is advantageous to carry out evaporation and calcination steps in another equipment like rotary calciner. Efforts have been directed for the engineering development of a Rotary Ball Kiln calciner. This paper highlights the important design features of the Rotary Ball Kiln Calciner for the radioactive waste. In this work, an attempt has been made to systematically evaluate the influence of process and design parameters. The results obtained on calcination will provide a design basis and rational methodology for the optimum utilization of these processes and equipment for volume reduction and calcination of the liquid waste

Treatment of wastewater containing dissolved metals by extraction-flotation

International Nuclear Information System (INIS)

Puget, Flavia Pereira

2002-02-01

In this work an alternative process for treating a wastewater containing dissolved metals (uranium and zirconium) is considered. In order to develop this work, a continuous separation unit, characterized by the association of solvent extraction and liquid-liquid flotation is used. Alamina 336 (a mixture of tri-octyl and tri-decyl amines) is used as extractant in the the extraction process, carried out inward the ejector. The splitting of the amine-water emulsion formed is carried out in a continuously operated flotation column (of approximately 2.5 L volume). The solvent extraction results showed that it is possible to reach an efficiency of about 95% for the uranium and zirconium extraction, for a metal in the feed concentration of 10 ppm and for a Q fa /Q fo ratio around 200. An efficiency of about 80% is reached in the flotation column when the liquid flowrate is equal 0.05 Lmin -1 and the air flowrate is equal 3.3 Lmin -1 . (author)

Solute redistribution studies in oxidised zirconium alloys

Energy Technology Data Exchange (ETDEWEB)

Khera, S K; Kale, G B; Gadiyar, H S [Bhabha Atomic Research Centre, Bombay (India). Metallurgy Div.

1977-01-01

Electron microprobe studies on solute distribution in oxide layers and in the regions near oxide metal interface have been carried out in the case of zircaloy-2 and zirconium binary alloys containing niobium, tin, iron, copper, chromium and nickel and oxidised in steam at 550 deg C. In the case of alloys having higher oxidation rates, the oxide of solute element was found to dissolve in ZrO/sub 2/ without any composition variation. However, for solute addition with limited solubility like Cr, Cu and Fe, solute enrichment at metal/oxide interface and depletion of the same matrix has been observed. The intensity profiles for nickel distribution were also found to be identical to Fe or Cr distribution. The mode of solute distribution has been discussed in relation to oxidation behaviour of these alloys.

Plasma arc melting of zirconium

International Nuclear Information System (INIS)

Tubesing, P.K.; Korzekwa, D.R.; Dunn, P.S.

1997-01-01

Zirconium, like some other refractory metals, has an undesirable sensitivity to interstitials such as oxygen. Traditionally, zirconium is processed by electron beam melting to maintain minimum interstitial contamination. Electron beam melted zirconium, however, does not respond positively to mechanical processing due to its large grain size. The authors undertook a study to determine if plasma arc melting (PAM) technology could be utilized to maintain low interstitial concentrations and improve the response of zirconium to subsequent mechanical processing. The PAM process enabled them to control and maintain low interstitial levels of oxygen and carbon, produce a more favorable grain structure, and with supplementary off-gassing, improve the response to mechanical forming

Optimization of Calcine Blending During Retrieval from Binsets

International Nuclear Information System (INIS)

Nelson, Lee Orville; Mohr, Charles Milton; Taylor, Dean Dalton

2000-01-01

This report documents a study performed during advanced feasibility studies for the INTEC Technology Development Facility (ITDF). The study was commissioned to provide information about functional requirements for the ITDF related to development of equipment and procedures for retrieving radioactive calcine from binset storage at the Idaho Nuclear Technology and Engineering Center (INTEC) at the Idaho National Engineering and Environmental Laboratory (INEEL). Calcine will be retrieved prior to treating it for permanent disposal in a national repository for high level waste. The objective this study was to estimate the degree of homogenization of the calcine that might be achieved through optimized retrieval and subsequent blending. Such homogenization has the potential of reducing the costs for treatment of the calcine and for qualifying of the final waste forms for acceptance at the repository. Results from the study indicate that optimized retrieval and blending can reduce the peak concentration variations of key components (Al, Zr, F) in blended batches of retrieved calcine. During un-optimized retrieval these variations are likely to be 81-138% while optimized retrieval can reduce them to the 5-10% range

Investigation of interaction of zirconium and hafnium tetrafluorides with strontium fluoride

International Nuclear Information System (INIS)

Ratnikova, I.D.; Korenev, Yu.M.; Novoselova, A.V.

1980-01-01

Diagrams of the condensated state of systems SrF 2 -EF 4 have been plotted, where E represents Zr, Hf. In these systems, three intermediate compounds of Sr 3 EF 10 , Sr 2 EF 8 and Sr EF 6 compositions are formed. All those compounds melt incongruently at temperatures of 982, 865 and 750 deg C, respectively - zirconium salt; at temperatures of 1000, 900 and 820 deg C - hafnium salts. Fluoro-metallates of composition 2:1, and 1:1, exist in two polymorphic forms. Tetrafluorides were found to dissolve in strontium fluoride: they form solid solutions having fluorite structure

Practical results of the MESA 1 line calcinator trial operation

International Nuclear Information System (INIS)

Napravnik, J.; Sazavsky, P.; Skaba, V.; Zahalka, F.; Vild, J.; Kulovany, J.

1987-01-01

Mobile calcination and cementation unit MESA 1 was designed and built by UJV Rez in cooperation with many enterprises, mainly with the Kralovopolske Strojirny Brno. This facility for direct fixation of liquid radioactive wastes was experimentally tested using model non-radioactive solutions and model and actual wastes from the Jaslovske Bohunice nuclear power plant. The calciner was run in trial operation at the Kralovopolske SAtrojirny Brno. A total of 1.3 m 3 of model solutions was processed into 180 kg of calcinate. The fixation of the calcinate in cement, the times of solidification and of hardening and the moisture content of concrete blocks were studied. The application was also tested of the calciner in drying ion exchangers from WWER-440 prior to their bituminization. Following the despatch of the cementation module to the Chernobyl nuclear power plant, the direct calcination module was tested at Dukovany together with an auxiliary module which makes possible self-contained calciner operation. Model non-radioactive solutions from the Dukovany nuclear power plant were treated containing H 3 BO 3 and NaNO 3 as main components. The usability in actual conditions of the mobile calcination and cementation unit for radioactive wastes was tested in a total of about 70 operating hours. (E.S.). 2 figs., 2 refs

Zirconium alloy barrier having improved corrosion resistance

International Nuclear Information System (INIS)

Adamson, R.B.; Rosenbaum, H.S.

1983-01-01

A nuclear fuel element for use in the core of a nuclear reactor has a composite cladding container having a substrate and a dilute zirconium alloy liner bonded to the inside surface of the substrate. The dilute zirconium alloy liner forms about 1 to about 20 percent of the thickness of the cladding and is comprised of zirconium and a metal selected from the group consisting of iron, chromium, iron plus chromium, and copper. The dilute zirconium alloy liner shields the substrate from impurities or fission products from the nuclear fuel material and protects the substrate from stress corrosion and stress cracking. The dilute zirconium alloy liner displays greater corrosion resistance, especially to oxidation by hot water or steam than unalloyed zirconium. The substrate material is selected from conventional cladding materials, and preferably is a zirconium alloy. (author)

Assessment of soda ash calcination treatment of Turkish trona ore

Directory of Open Access Journals (Sweden)

Gezer Sibel

2016-01-01

Full Text Available Trona is relatively rare, non-metallic mineral, Na2CO3 · NaHCO3 · 2H2O. The pure material contains 70.3% sodium carbonate and by calcination the excess CO2 and water can be driven off, yielding natural soda ash. The terms soda ash and sodium carbonate are used interchangeably. Trona calcining is a key process step in production of soda ash (sodium carbonate anhydrate from the relatively cheap trona ore. The calcination reaction may proceeds in a sequence of steps. Depending on the conditions, it may result in formation of either sodium carbonate monohydrate (Na2CO3 · H2O, sodium sesquicarbonate or weigschederite (Na2CO3 · 3NaHCO3. The Beypazarı Turkish trona deposit is the second largest deposit in the world with the content of 84% trona. The decomposition of trona appeared to be a single stage process across the temperature range studied (150-200 °C with the representative samples of different size fractions in the draught up metallurgical furnace. The optimum particle size and calcination time were −6.35 mm and 30 minutes, respectively, at calcination temperature of 175 °C in a metallurgical furnace. Microwave-induced dry calcination of trona was possible and 5 minutes of calcination time at a power level of 900 was sufficient for complete calcination of −6.35 mm feed. This includes short time calcinations with the goal of improving economics and simplifying the thermal process.

Zirconium behaviour in purex process solutions

International Nuclear Information System (INIS)

Shu, J.

1982-01-01

The extraction behaviour of zirconium, as fission product, in TBP/diluent- HNO 3 -H 2 O systems, simulating Purex solutions, is studied. The main purpose is to attain an increasing in the zirconium decontamination factor by adjusting the extraction parameters. Equilibrium diagram, TBP concentration, aqueous:organic ratio, salting-out effects and, uranium loading in the organic phase were the main factors studied. All these experiments had been made with zirconium in the 10 - 2 - 10 - 3 concentration range. The extractant degradation products influence uppon the zirconium behaviour was also verified. With the obtained data it was possible to introduce some modification in the standard Purex flow-sheet in order to obtain the uranium product with higher zirconium decontamination. (Author) [pt

Optimization of Calcine Blending During Retrieval From Binsets

International Nuclear Information System (INIS)

Taylor, D.D.; Mohr, C.M.; Nelson, L.O.

2000-01-01

This report documents a study performed during advanced feasibility studies for the INTEC Technology Development Facility (ITDF). The study was commissioned to provide information about functional requirements for the ITDF related to development of equipment and procedures for retrieving radioactive calcine from binset storage at the Idaho Nuclear Technology and Engineering Center (INTEC) at the Idaho National Engineering and Environmental Laboratory (INEEL). Calcine will be retrieved prior to treating it for permanent disposal in a national repository for high level waste. The objective this study was to estimate the degree of homogenization of the calcine that might be achieved through optimized retrieval and subsequent blending. Such homogenization has the potential of reducing the costs for treatment of the calcine and for qualifying of the final waste forms for acceptance at the repository. Results from the study indicate that optimized retrieval and blending can reduce the peak c oncentration variations of key components (Al, Zr, F) in blended batches of retrieved calcine. During un-optimized retrieval these variations are likely to be 81-138% while optimized retrieval can reduce them to the 5-10% range

Anisotropy of mechanical properties of zirconium and zirconium alloys

International Nuclear Information System (INIS)

Medrano, R.E.

1975-01-01

In studies of technological applications of zirconium to fuel elements of nuclear reactor, it was found that the use of plasticity equations for isotropic materials is not in agreement with experimental results, because of the strong anisotropy of zirconium. The present review describes recent progress on the knowledge of the influence of anisotropy on mechanical properties, after Douglass' review in 1971. The review was written to be selfconsistent, changing drastically the presentation of some of the referenced papers. It is also suggested some particular experiments to improve developments in this area

New solvent extraction process for zirconium and hafnium

International Nuclear Information System (INIS)

Takahashi, M.; Katoh, Y.; Miyazaki, H.

1984-01-01

The authors' company developed a new solvent extraction process for zirconium and hafnium separation, and started production of zirconium sponge by this new process in September 1979. The process utilizes selective extraction of zirconium oxysulfate using high-molecular alkyl amine, and has the following advantages: 1. This extraction system has a separation factor as high as 10 to 20 for zirconium and hafnium in the range of suitable acid concentration. 2. In the scrubbing section, removal of all the hafnium that coexists with zirconium in the organic solvent can be effectively accomplished by using scrubbing solution containing hafnium-free zirconium sulfate. Consequently, hafnium in the zirconium sponge obtained is reduced to less than 50 ppm. 3. The extractant undergoes no chemical changes but is very stable for a long period. In particular, its solubility in water is small, about 20 ppm maximum, posing no environmental pollution problems such as are often caused by other process raffinates. At the present time, the zirconium and hafnium separation operation is very stable, and zirconium sponge made by this process can be applied satisfactorily to nuclear reactors

Hot isostatically-pressed aluminosilicate glass-ceramic with natural crystalline analogues for immobilizing the calcined high-level nuclear waste at the Idaho Chemical Processing Plant

International Nuclear Information System (INIS)

Raman, S.

1993-12-01

The additives Si, Al, MgO, P 2 O 5 were mechanically blended with fluorinelsodium calcine in varying proportions. The batches were vacuum sealed in stainless steel canisters and hot isostatically pressed at 20,000 PSI and 1000 C for 4 hours. The resulting suite of glass-ceramic waste forms parallels the natural rocks in microstructural and compositional heterogeneity. Several crystalline phases ar analogous in composition and structure to naturally occurring minerals. Additional crystalline phases are zirconia and Ca-Mg borate. The glasses are enriched in silica and alumina. Approximately 7% calcine elements occur dissolved in this glass and the total glass content in the waste forms averages 20 wt%. The remainder of the calcine elements are partitioned into crystalline phases at 75 wt% calcine waste loading. The waste forms were tested for chemical durability in accordance with the MCC1-test procedure. The leach rates are a function of the relative proportions of additives and calcine, which in turn influence the composition and abundances of the glass and crystalline phases. The DOE leach rate criterion of less than 1 g/m 2 -day is met by all the elements B, Cs and Na are increased by lowering the melt viscosity. This is related to increased crystallization or devitrification with increases in MgO addition. This exploratory work has shown that the increases in waste loading occur by preferred partitioning of the calcine components among crystalline and glass phases. The determination of optimum processing parameters in the form of additive concentration levels, homogeneous blending among the components, and pressure-temperature stabilities of phases must be continued to eliminate undesirable effects of chemical composition, microstructure and glass devitrification

Modeling of calcination of single kaolinitic clay particle

DEFF Research Database (Denmark)

Gebremariam, Abraham Teklay; Yin, Chungen; Rosendahl, Lasse

The present work aims at modeling of the calcination (dehydroxylation) process of clay particles, specifically kaolinite, and its thermal transformation. For such purpose, 1D single particle calcination model was developed based on the concept of shrinking core model to assess the dehydroxylation...

Fine-grained zirconium-base material

Science.gov (United States)

Van Houten, G.R.

1974-01-01

A method is described for making zirconium with inhibited grain growth characteristics, by the process of vacuum melting the zirconium, adding 0.3 to 0.5% carbon, stirring, homogenizing, and cooling. (Official Gazette)

Microhardness and microplasticity of zirconium nitride

International Nuclear Information System (INIS)

Neshpor, V.S.; Eron'yan, M.A.; Petrov, A.N.; Kravchik, A.E.

1978-01-01

To experimentally check the concentration dependence of microhardness of 4 group nitrides, microhardness of zirconium nitride compact samples was measured. The samples were obtained either by bulk saturation of zirconium iodide plates or by chemical precipitation from gas. As nitrogen content decreased within the limits of homogeneity of zirconium nitride samples where the concentration of admixed oxygen was low, the microhardness grew from 1500+-100 kg/mm 2 for ZrNsub(1.0) to 27000+-100 kg/mm 2 for ZrNsub(0.78). Microplasticity of zirconium nitride (resistance to fracture) decreased, as the concentration of nitrogen vacancies was growing

Calcination of kaolinite clay particles for cement production

DEFF Research Database (Denmark)

Gebremariam, Abraham Teklay; Yin, Chungen; Rosendahl, Lasse

2014-01-01

Kaolinite rich clay particles calcined under certain conditions can attain favorable pozzolanic properties and can be used to substitute part of the CO2 intensive clinker in cement production. To better guide calcination of a clay material, a transient one-dimensional single particle model...

Zirconium

Science.gov (United States)

Bedinger, G.M.

2013-01-01

Zirconium is the 20th most abundant element in the Earth’s crust. It occurs in a variety of rock types and geologic environments but most often in igneous rocks in the form of zircon (ZrSiO4). Zircon is recovered as a coproduct of the mining and processing of heavy mineral sands for the titanium minerals ilmenite and rutile. The sands are formed by the weathering and erosion of rock containing zircon and titanium heavy minerals and their subsequent concentration in sedimentary systems, particularly in coastal environments. A small quantity of zirconium, less than 10 kt/a (11,000 stpy), compared with total world production of 1.4 Mt (1.5 million st) in 2012, was derived from the mineral baddeleyite (ZrO2), produced from a single source in Kovdor, Russia.

Extractive metallurgy of zirconium--1945 to the present

International Nuclear Information System (INIS)

Franklin, D.G.; Adamson, R.B.

1984-01-01

Although the history of the reduction of zirconium dates from 1824 and the first ductile zirconium metal was produced in the laboratory in 1914, modern reduction practice was pioneered by the U.S. Bureau of Mines starting in 1945. This paper reviews the history of the extractive metallurgy of zirconium from the early work of W. J. Kroll and co-workers at the Bureau of Mines in Albany, Ore., through the commercial development of the production of reactor-grade zirconium metal which was spurred by the requirements of the Naval Reactor Program and the development of commercial nuclear power. Technical subjects covered include processes for opening the ore, zirconium-hafnium separation, chlorination of zirconium oxide, reduction processes, and electrowinning of zirconium metal. Proposed new processes and process modifications are reviewed

Effects of rapid calcination on properties of calcium-based sorbents

International Nuclear Information System (INIS)

Yan, Chang-Feng; Grace, John R.; Lim, C. Jim

2010-01-01

The calcination process may influence subsequent fragmentation, sintering and swelling when CaO derived from limestone acts as a CO 2 or SO 2 -sorbent in combustion, gasification and reforming. Sorbent properties are affected by CO 2 partial pressure, total pressure, temperature, heating rate, impurities and sample size. In this study, the effect of calcination heating rate was investigated based on an electrically heated platinum foil. The effects of heating rate (up to 800 C/s), calcination temperature (700-950 C), particle size (90-180 μm) and sweep gas velocity were investigated. Higher initial heating rates led to lower extents of limestone calcination, but the extents of carbonation of the resulting CaO were similar to each other. Calcium utilization declined markedly during carbonation or sulphation of CaO after calcination by rapid heating. Experimental results show that carbonation and calcium utilization were most effective for carbonation temperatures between 503 and 607 C. Increasing the extent of calcination is not the best way to improve overall calcium utilization due to the vast increase in energy consumption. (author)

CSER 99-001: PFP LAB Dentirating calciner

International Nuclear Information System (INIS)

MILLER, E.M.; DOBBIN, K.D.

1999-01-01

A criticality safety evaluation report was prepared for the Plutonium Finishing Plant (PFP) laboratory denigrating calciner, located in Glovebox 188-1, that converts Pu(NO 3 ) 4 solutions to the high fired stable oxide PuO 2 . Fissile mass limits and volume limits are set for the glovebox for testing operations and training operators using only nitric acid feed to a plutonium oxide bed in the calciner

Purification of zirconium concentrates

International Nuclear Information System (INIS)

Brown, A.E.P.

1976-01-01

A commercial grade ZrO 2 and an ammonium uranate (yellow cake) are obtained from the caldasito ore processing. This ore is found in the Pocos de Caldas Plateau, State of Minas Gerais, Brazil. Caldasito is an uranigerous zirconium ore, a mixture of zircon and baddeleyite and contains 60% ZrO 2 and 0,3% U 3 O 8 . The chemical opening of the ore was made by alkaline fusion with NaOH at controlled temperature. The zirconium-uranium separation took place by a continuous liquid-liquid extraction in TBP-varsol-HNO 3 -H 2 O system. The raffinate containing zirconium + impurities (aluminium, iron and titanium) was purified by an ion exchange operation using a strong cationic resin [pt

Determination of zirconium by fluoride ion selective electrode

International Nuclear Information System (INIS)

Mahanty, B.N.; Sonar, V.R.; Gaikwad, R.; Raul, S.; Das, D.K.; Prakash, A.; Afzal, Md.; Panakkal, J.P.

2010-01-01

Full text: Zirconium is used in a wide range of applications including nuclear clad, catalytic converters, surgical appliances, metallurgical furnaces, superconductors, ceramics, lamp filaments, anti corrosive alloys and photographical purposes. Irradiation testing of U-Zr and U-Pu-Zr fuel pins has also demonstrated their feasibility as fuel in liquid metal reactors. Different methods that are employed for the determination of zirconium are spectrophotometry, potentiometry, neutron activation analysis and mass spectrometry. Ion-selective electrode (ISE), selective to zirconium ion has been studied for the direct potentiometric measurements of zirconium ions in various samples. In the present work, an indirect method has been employed for the determination of zirconium in zirconium nitrate sample using fluoride ion selective electrode. This method is based on the addition of known excess amount of fluoride ion to react with the zirconium ion to produce zirconium tetra fluoride at about pH 2-3, followed by determination of residual fluoride ion selective electrode. The residual fluoride ion concentrations were determined from the electrode potential data using calibration plot. Subsequently, zirconium ion concentrations were determined from the concentration of consumed fluoride ions. A precision of about 2% (RSD) with the mean recovery of more than 94% has been achieved for the determination of zirconium at the concentration of 4.40 X 10 -3 moles lit -1

Fluidized bed calciner

International Nuclear Information System (INIS)

Sheely, W.F.

1986-01-01

A unique way to convert radioactive scrap into useful nuclear fuel products was developed for the Department of Energy at Hanford. An advanced, fluidized bed calciner is used to convert metallic nitrate scrap or waste solutions into benign, solid and gaseous products. There are broad potential applications of this concept beyond those in the nuclear industry

Thermofluency in zirconium alloys

International Nuclear Information System (INIS)

Orozco M, E.A.

1976-01-01

A summary is presented about the theoretical and experimental results obtained at present in thermofluency under radiation in zirconium alloys. The phenomenon of thermofluency is presented in a general form, underlining the thermofluency at high temperature because this phenomenon is similar to the thermofluency under radiation, which ocurrs in zirconium alloys into the operating reactor. (author)

Properties of Formula 127 glass prepared with radioactive zirconia calcine

International Nuclear Information System (INIS)

Staples, B.A.; Pavlica, D.A.; Cole, H.S.

1982-09-01

Formula 127 glass has been developed to immobilize ICPP zirconia calcine. This glass has been prepared remotely on a laboratory scale basis with actual radioactive zirconia calcine retrieved after ten years of storage from Bin Set 2. The aqueous leachability of the glass produced was investigated and compared through application of the MCC-1, MCC-2 and Soxhlet leach tests with that of Formula 127 glass prepared with simulated calcine. The solid state properties of the glasses prepared with actual and simulated calcines were also measured by electron spectroscopy for chemical analysis (ESCA) and scanning electron microscopy energy dispersive x-ray (SEM-EDX). Based on the application of these leaching tests and analysis techniques the properties measured in this study are similar for 127 glass prepared with either simulated or radioactive calcine. 13 figures, 16 tables

Quantitative analysis of nickel in zirconium and zircaloy; Dosage du nickel dans le zirconium et dans le zircaloy

Energy Technology Data Exchange (ETDEWEB)

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

1957-07-01

A rapid spectrophotometric has been developed for determination of 10 to 1000 ppm of Ni in zirconium and zircaloy using dimethylglyoxime. Iron, copper, tin and chromium, do not interfere at the concentration usually present in zirconium and its alloys. (author) [French] On determine colorimetriquenent 10 a 1000 ppm de Ni dans le zirconium et le zircaloy par photo colorimetrie a 440 m{mu} de la dimethylglyoxime nickelique. Le dosage est rapide. Le fer, le cuivre, l'etain, le chrome ne genent pas aux concentrations habituellement rencontrees dans le zirconium et ses alliages. (auteur)

40 CFR 721.9973 - Zirconium dichlorides (generic).

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Zirconium dichlorides (generic). 721... Substances § 721.9973 Zirconium dichlorides (generic). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances identified generically as zirconium dichlorides (PMNs P...

Molten salt scrubbing of zirconium or hafnium tetrachloride

International Nuclear Information System (INIS)

Lee, E.D.; McLaughlin, D.F.

1990-01-01

This patent describes a continuous process for removing impurities of iron or aluminum chloride or both from vaporous zirconium or hafnium chloride or both. It comprises: introducing impure zirconium or hafnium chloride vapor or both into a middle portion of an absorbing column containing a molten salt phase, the molten salt phase absorbing the impurities of iron or aluminum chloride or both to produce chloride vapor stripped of zirconium or hafnium chloride; introducing sodium or potassium chloride or both into a top portion of the column; controlling the top portion of the column to between 300--375 degrees C.; heating a bottom portion of the column to 450--550 degrees C. To vaporize zirconium chloride or hafnium chloride or hafnium and zirconium chloride from the molten salt; withdrawing molten salt substantially free of zirconium and hafnium chloride from the bottom portion of the column; and withdrawing zirconium chloride or hafnium chloride or hafnium and zirconium chloride vapor substantially free of impurities of iron and aluminum chloride from the top of the column

Advances in zirconium technology for nuclear reactor application

International Nuclear Information System (INIS)

Ganguly, C.

2002-01-01

Zirconium alloys are extensively used as a material for cladding nuclear fuels and for making core structurals of water-cooled nuclear power reactors all over the world for generation of nearly 16 percent of the worlds electricity. Only four countries in the world, namely France, USA, Russia and India, have large zirconium industry and capability to manufacture reactor grade zirconium sponge, a number of zirconium alloys and a wide variety of structural components for water cooled nuclear reactor. The present paper summarises the status of zirconium technology and highlights the achievement of Nuclear Fuel Complex during the last ten years in developing a wide variety of zirconium alloys and components for water-cooled nuclear power programme

Optimization of Calcine Blending During Retrieval From Binsets; TOPICAL

International Nuclear Information System (INIS)

Taylor, D.D.; Mohr, C.M.; Nelson, L.O.

2000-01-01

This report documents a study performed during advanced feasibility studies for the INTEC Technology Development Facility (ITDF). The study was commissioned to provide information about functional requirements for the ITDF related to development of equipment and procedures for retrieving radioactive calcine from binset storage at the Idaho Nuclear Technology and Engineering Center (INTEC) at the Idaho National Engineering and Environmental Laboratory (INEEL). Calcine will be retrieved prior to treating it for permanent disposal in a national repository for high level waste. The objective this study was to estimate the degree of homogenization of the calcine that might be achieved through optimized retrieval and subsequent blending. Such homogenization has the potential of reducing the costs for treatment of the calcine and for qualifying of the final waste forms for acceptance at the repository. Results from the study indicate that optimized retrieval and blending can reduce the peak c oncentration variations of key components (Al, Zr, F) in blended batches of retrieved calcine. During un-optimized retrieval these variations are likely to be 81-138% while optimized retrieval can reduce them to the 5-10% range

Applications for zirconium and columbium alloys

International Nuclear Information System (INIS)

Condliff, A.F.

1986-01-01

Currently, zirconium and columbium are used in a wide range of applications, overlapping only in the field of corrosion control. As a construction material, zirconium is primarily used by the nuclear power industry. The use of zirconium in the chemical processing industry (CPI) is, however, increasing steadily. Columbian alloys are primarily applied as superconducting alloys for research particle accelerators and fusion generators as well as in magnetic resonance imaging for medical diagnosis

Calcinating petroleum coke in a furnace with a rotating hearth

Energy Technology Data Exchange (ETDEWEB)

Akhmetov, M M; Ezhov, B M; Galeeva, Z G; Goriunov, V S; Karpinskaia, N N; Zaitseva, S A

1980-01-01

A scheme is described for an industrial device with a bottom furnace for calcinating coke from slow coking. The consumption and operational indicators of the process during the calcination of standard and needle cokes are given, together with data on the quality of dry and calcinated cokes under different conditions. The basic drawbacks in the operation of the device are described, and measures are proposed for increasing its operational effectiveness.

Measurement of total dissolved solids using electrical conductivity

International Nuclear Information System (INIS)

Ray, Vinod K.; Jat, J.R.; Reddy, G.B.; Balaji Rao, Y.; Phani Babu, C.; Kalyanakrishnan, G.

2017-01-01

Total dissolved solids (TDS) is an important parameter for the disposal of effluents generated during processing of different raw materials like Magnesium Di-uranate (MDU), Heat Treated Uranium Peroxide (HTUP), Sodium Di-uranate (SDU) in Uranium Extraction plant and Washed and Dried Frit (WDF) in Zirconium Extraction Plant. The present paper describes the use of electrical conductivity for determination of TDS. As electrical conductivity is matrix dependent property, matrix matched standards were prepared for determination of TDS in ammonium nitrate solution (AN) and mixture of ammonium nitrate and ammonium sulphate (AN/AS) and results were found to be in good agreement when compared with evaporation method. (author)

The development of zirconium alloy and its manufacturing

International Nuclear Information System (INIS)

Yuan Gaihuan; Yue Qiang

2015-01-01

Nuclear power which acts as one of low-carbon energy resources is the most realistic in large-scale application. It is also the preferred choice for many countries to develop energy resources and optimize its structure. Zirconium alloy is a key structural material for nuclear power plant fuel assemblies and cladding tubes of zirconium alloy are often referred as the first safeguard to nuclear power safety. With the development of nuclear power, three kinds of zirconium alloys Zr-Sn, Zr-Nb, Zr-Sn-Nb and with the representative products of Zr-4, M5, Zirlo respectively are developed and widely applied. Because of its severe operating environment and influence to nuclear safety, the requirements to zirconium alloys for physical and chemical properties, nuclear capability, tolerance and surface quality are very strict. The in-depth research and its manufacture capability become one of the main barriers for many countries who are developing the nuclear energy. In recent years, a stated-owned company, State Nuclear Bao Ti Zirconium Industry Company ('SNZ' for short) as well as National R and D Center for Nuclear Grade Zirconium material, is founded to meet the requirement of the rapid development of China's nuclear power industry. SNZ is dedicated for the fabrication and the research of nuclear grade zirconium products. After the successful completion of technology transfer of manufacturing for production chain and fully grasped of the manufacturing technology for the nuclear grade zirconium sponge through zirconium alloy tube, rod and strip products. National R and D Center for Nuclear Grade Zirconium material is cooperating with universities, nuclear energy research and design institutes and the owners of nuclear power plant to develop new zirconium alloy of self-owned brand. Through the selection of components, in-process testing and product inspection, four kinds of new zirconium alloys owns better performance than currently commercialized M5, Zirlo etc

Leaching properties and chemical compositions of calcines produced at the Idaho Chemical Processing Plant

International Nuclear Information System (INIS)

Staples, B.A.; Paige, B.E.; Rhodes, D.W.; Wilding, M.W.

1980-01-01

No significant chemical differences were determined between retrieved and fresh calcine based on chemical and spectrochemical analyses. Little can be derived from the amounts of the radioisotopes present in the retrieved calcine samples other than the ratios of strontium-90 to cesium-137 are typical of aged fission product. The variations in concentrations of radionuclides within the composite samples of each bin also reflect the differences in compositions of waste solutions calcined. In general the leaching characteristics of both calcines by distilled water are similar. In both materials the radionuclides of cesium and strontium were selectively leached at significant rates, although cesium leached much more completely from the alumina calcine than from the zirconia calcine. Cesium and strontium are probably contained in both calcines as nitrate salts and also as fluoride salts in zirconia calcine, all of which are at least slightly soluble in water. Radionuclides of cerium, ruthenium, and plutonium in both calcines were highly resistant to leaching and leached at rates similar to or less than those of the matrix elements. These elements exist as polyvalent metal ions in the waste solutions before calcination and they probably form insoluble oxides and fluorides in the calcine. The relatively slow leaching of nitrate ion from zirconia calcine and radiocesium from both calcines suggests that the calcine matrix in some manner prevents complete or immediate contact of the soluble ions with water. Whether radiostrontium forms slightly fluoride salts or forms nitrate salts which are protected in the same manner as radiocesium is unknown. Nevertheless, selective leaching of cesium and strontim is retarded in some manner by the calcine matrix

Oxidized zirconium on ceramic; Catastrophic coupling.

Science.gov (United States)

Ozden, V E; Saglam, N; Dikmen, G; Tozun, I R

2017-02-01

Oxidized zirconium (Oxinium™; Smith & Nephew, Memphis, TN, USA) articulated with polyethylene in total hip arthroplasty (THA) appeared to have the potential to reduce wear dramatically. The thermally oxidized metal zirconium surface is transformed into ceramic-like hard surface that is resistant to abrasion. The exposure of soft zirconium metal under hard coverage surface after the damage of oxidized zirconium femoral head has been described. It occurred following joint dislocation or in situ succeeding disengagement of polyethylene liner. We reported three cases of misuse of Oxinium™ (Smith & Nephew, Memphis, TN, USA) heads. These three cases resulted in catastrophic in situ wear and inevitable failure although there was no advice, indication or recommendation for this use from the manufacturer. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

Electrochemical-metallothermic reduction of zirconium in molten salt solutions

International Nuclear Information System (INIS)

McLaughlin, D.F.; Talko, F.

1990-01-01

This patent describes a method for separating hafnium from zirconium of the type wherein a feed containing zirconium and hafnium chlorides is prepared from zirconium-hafnium chloride and the feed is introduced into a distillation column, which distillation column has a reboiler connected at the bottom and a reflux condenser connected at the top and wherein a hafnium chloride enriched stream is taken from the top of the column and a zirconium enriched chloride stream is taken from the bottom of the column. It comprises: reducing the zirconium enriched chloride stream taken from the distillation column to metal by electrochemically reducing an alkaline earth metal in a molten salt bath with the molten salt in the molten salt bath consisting essentially of a mixture of at least one alkali metal chloride and at least one alkaline earth metal chloride and zirconium chloride, with the reduced alkaline earth metal reacting with the zirconium chloride to produce zirconium metal and alkaline earth metal chloride

Calcined Waste Storage at the Idaho Nuclear Technology and Engineering Center

Energy Technology Data Exchange (ETDEWEB)

M. D. Staiger

2007-06-01

This report provides a quantitative inventory and composition (chemical and radioactivity) of calcined waste stored at the Idaho Nuclear Technology and Engineering Center. From December 1963 through May 2000, liquid radioactive wastes generated by spent nuclear fuel reprocessing were converted into a solid, granular form called calcine. This report also contains a description of the calcine storage bins.

High Temperature Calcination - MACT Upgrade Equipment Pilot Plant Test

Energy Technology Data Exchange (ETDEWEB)

Richard D. Boardman; B. H. O& #39; Brien; N. R. Soelberg; S. O. Bates; R. A. Wood; C. St. Michel

2004-02-01

About one million gallons of acidic, hazardous, and radioactive sodium-bearing waste are stored in stainless steel tanks at the Idaho Nuclear Technology and Engineering Center (INTEC), which is a major operating facility of the Idaho National Engineering and Environmental Laboratory. Calcination at high-temperature conditions (600 C, with alumina nitrate and calcium nitrate chemical addition to the feed) is one of four options currently being considered by the Department of Energy for treatment of the remaining tank wastes. If calcination is selected for future processing of the sodium-bearing waste, it will be necessary to install new off-gas control equipment in the New Waste Calcining Facility (NWCF) to comply with the Maximum Achievable Control Technology (MACT) standards for hazardous waste combustors and incinerators. This will require, as a minimum, installing a carbon bed to reduce mercury emissions from their current level of up to 7,500 to <45 {micro}g/dscm, and a staged combustor to reduce unburned kerosene fuel in the off-gas discharge to <100 ppm CO and <10 ppm hydrocarbons. The staged combustor will also reduce NOx concentrations of about 35,000 ppm by 90-95%. A pilot-plant calcination test was completed in a newly constructed 15-cm diameter calciner vessel. The pilot-plant facility was equipped with a prototype MACT off-gas control system, including a highly efficient cyclone separator and off-gas quench/venturi scrubber for particulate removal, a staged combustor for unburned hydrocarbon and NOx destruction, and a packed activated carbon bed for mercury removal and residual chloride capture. Pilot-plant testing was performed during a 50-hour system operability test January 14-16, followed by a 100-hour high-temperature calcination pilot-plant calcination run January 19-23. Two flowsheet blends were tested: a 50-hour test with an aluminum-to-alkali metal molar ratio (AAR) of 2.25, and a 50-hour test with an AAR of 1.75. Results of the testing

Problems of zirconium metal production in Czechoslovakia

International Nuclear Information System (INIS)

Vareka, J.; Vaclavik, E.

1975-01-01

The problems are summed up of the production and quality control of zirconium sponge. A survey is given of industrial applications of zirconium in form of pure metal or alloys in nuclear power production, ferrous and non-ferrous metallurgy, chemical engineering and electrical engineering. A survey is also presented of the manufacture of zirconium metal in advanced capitalist countries. (J.B.)

Criticality safety analysis of a calciner exit chute

International Nuclear Information System (INIS)

Haught, C.F.; Basoglu, B.; Brewer, R.W.; Hollenback, D.F.; Wilkinson, A.D.; Dodds, H.L.

1994-01-01

Calcination of uranyl nitrate into uranium oxide is part of normal operations of some enrichment plants. Typically, a calciner discharges uranium oxide powder (U 3 O 8 ) into an exit chute that directs the powder into a receiving can located in a glove box. One possible scenario for a criticality accident is the exit chute becoming blocked with powder near its discharge. The blockage restricts the flow of powder causing the exit chute to become filled with the powder. If blockage does occur, the height of the powder could reach a level that would not be safe from a criticality point of view. In this analysis, the subcritical height limit is examined for 98% enriched U 3 O 8 in the exit chute with full water reflection and optimal water moderation. The height limit for ensuring criticality safety during such an accumulation is 28.2 cm above the top of the discharge pipe at the bottom of the chute. Chute design variations are also evaluated with full water reflection and optimal water moderation. Subcritical configurations for the exit chute variation are developed, but the configurations are not safe when combined with the calciner. To ensure criticality safety, modifications must be made to the calciner tube or safety measures must be implemented if these designs are to be utilized with 98% enriched material. A geometrically safe configuration for the exit chute is developed for a blockage of 20% enriched powder with full water reflection and optimal water moderation, and this configuration is safe when combined with the existing calciner

Phase Transformations in a Uranium-Zirconium Alloy containing 2 weight per cent Zirconium

Energy Technology Data Exchange (ETDEWEB)

Lagerberg, G

1961-04-15

The phase transformations in a uranium-zirconium alloy containing 2 weight percent zirconium have been examined metallographically after heat treatments involving isothermal transformation of y and cooling from the -y-range at different rates. Transformations on heating and cooling have also been studied in uranium-zirconium alloys with 0.5, 2 and 5 weight per cent zirconium by means of differential thermal analysis. The results are compatible with the phase diagram given by Howlett and Knapton. On quenching from the {gamma}-range the {gamma} phase transforms martensitically to supersaturated a the M{sub S} temperature being about 490 C. During isothermal transformation of {gamma} in the temperature range 735 to 700 C {beta}-phase is precipitated as Widmanstaetten plates and the equilibrium structure consists of {beta} and {gamma}{sub 1}. Below 700 C {gamma} transforms completely to Widmanstaetten plates which consist of {beta} above 660 C and of a at lower temperatures. Secondary phases, {gamma}{sub 2} above 610 C and {delta} below this temperature, are precipitated from the initially supersaturated Widmanstaetten plates during the isothermal treatments. At and slightly below 700 C the cooperative growth of |3 and {gamma}{sub 2} is observed. The results of isothermal transformation are summarized in a TTTdiagram.

The fluorimetric titration of zirconium in the ppm-range

International Nuclear Information System (INIS)

Linden, W.E. von der; Boef, G. den; Ozinga, W.

1976-01-01

A fluorimetric titration of zirconium(IV) with EDTA is proposed. The fluorescence intensity of the zirconium-morin complex is used to indicate the end-point. More than twenty other cations were investigated and it was found that they did not interfere, neither did common anions. Mercury(II) can only be tolerated in amount not exceeding that of zirconium. Bismuth(III) interferes and hafnium(IV0 is titrated together with zirconium. The relative standard deviation of the titration of 10ml of a solution containing 1 ppm of zirconium does not exceed 1.5%

Corrosion Behavior and Oxide Properties of Zr-Nb-Cu and Zr-Nb-Sn Alloy in High Dissolved Hydrogen Primary Water Chemistry

Energy Technology Data Exchange (ETDEWEB)

Lee, Yun Ju; Kim, Tae Ho; Kim, Ji Hyun [UNIST, Ulsan (Korea, Republic of)

2016-05-15

The water-metal interface is regarded as rate-controlling site governing the rapid oxidation transition in high burn-up fuel. And the zirconium oxide is made in water-metal interface and its structure and phase do an important role in terms of oxide properties. During oxidation process, the protective tetragonal oxide layer develops at the interface due to accumulated high stress during oxide growth, and it turns into non-protective monoclinic oxide with increasing oxide thickness, thus decreasing the stress. It has been reported that Nb addition was proven to be very beneficial for increasing the corrosion resistance of the zirconium alloys. From a more recent study, Cu addition in Nb containing Zirconium alloy was reported to be effective for increasing corrosion resistance in water containing B and Li. According to the previous research conducted, Zr-Nb-Cu shows better corrosion resistance than Zircaloy-4. The dissolved hydrogen (DH) concentration is the key issue of primary water chemistry, and the effect of DH concentration on the corrosion rate of nickel based alloy has been researched. However, the effect of DH on the zirconium alloy corrosion mechanism was not fully investigated. In this study, the weight gain measurement, FIB-SEM analysis, and Raman spectroscopic measurement were conducted to investigate the effects of dissolved hydrogen concentration and the chemical composition on the corrosion resistance and oxide phase of Zr-Nb-Cu alloy and Zr-Nb-Sn alloy after oxidizing in a primary water environment for 20 d. The corrosion rate of Zr-Nb-Cu alloy is slow, when it is compared to Zr-Nb-Sn alloy. In SEM images, the oxide thickness of Zr-Nb-Cu alloy is measured to be around 1.06 μm it of Zr-Nb-Sn alloy is measured to be 1.15 μm. It is because of the Segregation made by Sn solute element when Sn solute element oxidized. And according to ex situ Raman spectra, Zr-Nb-Cu alloy oxide has more tetragonal zirconium oxide fraction than Zr-Nb-Sn alloy oxide.

SEPARATING HAFNIUM FROM ZIRCONIUM

Science.gov (United States)

Lister, B.A.J.; Duncan, J.F.

1956-08-21

A dilute aqueous solution of zirconyl chloride which is 1N to 2N in HCl is passed through a column of a cation exchange resin in acid form thereby absorbing both zirconium and associated hafnium impurity in the mesin. The cation exchange material with the absorbate is then eluted with aqueous sulfuric acid of a O.8N to 1.2N strength. The first portion of the eluate contains the zirconium substantially free of hafnium.

Spectrophotometric titration of zirconium in siliceous materials

International Nuclear Information System (INIS)

Sugawara, K.F.; Su, Y.-S.; Strzegowski, W.R.

1978-01-01

An accurate and selective complexometric titration procedure based upon a spectrophotometrically detected end-point has been developed for the determination of zirconium in glasses, glass-ceramics and refractories. A p-bromomandelic acid separation step for zirconium imparts excellent selectivity to the procedure. The method is particularly important for the 1 to 5% concentration range where a simple, accurate and selective method for the determination of zirconium has been lacking. (author)

Wear and chemistry of zirconium-silicate, aluminium-silicate and zirconium-aluminium-silicate glasses in alkaline medium

International Nuclear Information System (INIS)

Rouse, C.G.; Lemos Guenaga, C.M. de

1984-01-01

A study of the chemical durability, in alkaline solutions, of zirconium silicate, aluminium silicate, zirconium/aluminium silicate glasses as a function of glass composition is carried out. The glasses were tested using standard DIN-52322 method, where the glass samples are prepared in small polished pieces and attacked for 3 hours in a 800 ml solution of 1N (NaOH + NA 2 CO 3 ) at 97 0 C. The results show that the presence of ZrO 2 in the glass composition increases its chemical durability to alkaline attack. Glasses of the aluminium/zirconium silicate series were melted with and without TiO 2 . It was shown experimentally that for this series of glasses, the presence of both TiO 2 and ZrO 2 gave better chemical durability results. However, the best overall results were obtained from the simpler zirconium silicate glasses, where it was possible to make glasses with higher values of ZrO 2 . (Author) [pt

Kinetic Study of Calcination of Jakura Limestone Using Power Rate ...

African Journals Online (AJOL)

National Research Institute for Chemical Technology, P.M. B 1052, Zaria, ... calcination of Jakura limestone was also found to be first order reaction with respect to CaCO3 ... Keywords: Jakura, limestone, calcination, kinetics, power law model.

Study for the chlorination of zirconium oxide

International Nuclear Information System (INIS)

Seo, E.S.M.; Takiishi, H.; Paschoal, J.O.A.; Andreoli, M.

1990-12-01

In the development of new ceramic and metallic materials the chlorination process constitutes step in the formation of several intermediate compounds, such as metallic chlorides, used for the production of high, purity raw materials. Chlorination studies with the aim of fabrication special zirconium-base alloys have been carried out at IPEN. Within this program the chlorination technique has been used for zirconium tetrachloride production from zirconium oxide. In this paper some relevant parameters such as: time and temperature of reaction, flow rate of chloride gas and percentage of the reducing agent which influence the efficiency of chlorination of zirconium oxide are evaluated. Thermodynamical aspects about the reactions involved in the process are also presented. (author)

Ductile zirconium powder by hydride-dehydride process

Energy Technology Data Exchange (ETDEWEB)

Krishnan, T S [BHABHA ATOMIC RESEARCH CENTRE, BOMBAY (INDIA); CHAUDHARY, S [NUCLEAR FUEL COMPLEX, HYDERABAD (INDIA)

1976-09-01

The preparation of ductile zirconium powder by the hydride-dehydride process has been described. In this process massive zirconium obtained from Kroll reduction of ZrCl/sub 4/ is first rendered brittle by hydrogenation and the hydride crushed and ground in a ball mill to the required particle size. Hydrogen is then hot vacuum extracted to yield the metal powder. The process has been successfully employed for the production of zirconium powders with low oxygen content and having hardness values in the range of 115-130 BHN, starting from a zirconium sponge of 100-120 BHN hardness. Influence of surface characteristics of the starting metal on its hydriding behaviour has been studied and the optimum hydriding-dehydriding conditions established.

Joint titrimetric determination of zirconium and hafnium

International Nuclear Information System (INIS)

Vazquez, Cristina; Botbol, Moises; Bianco de Salas, G.N.; Cornell de Casas, M.I.

1980-01-01

A method for the joint titrimetric determination of zirconium and hafnium, which are elements of similar chemical behaviour, is described. The disodic salt of the ethylendiaminetetracetic acid (EDTA) is used for titration, while xilenol orange serves as final point indicator. Prior to titration it is important to evaporate with sulfuric acid, the solution resulting from the zirconium depolymerization process, to adjust the acidity and to eliminate any interferences. The method, that allows the quick and precise determination of zirconium and hafnium in quantities comprised between 0.01 and mg, was applied to the analysis of raw materials and of intermediate and final products in the fabrication of zirconium sponge and zircaloy. (M.E.L.) [es

Physical and chemical characterization of synthetic calcined sludge

International Nuclear Information System (INIS)

Slates, R.V.; Mosley, W.C. Jr.; Tiffany, B.; Stone, J.A.

1982-03-01

Calcined synthetic sludge was chemically characterized in support of engineering studies to design a processing plant to solidify highly radioactive waste at the Savannah River Plant. An analytical technique is described which provides quantitative data by mass spectrometric analysis of gases evolved during thermogravimetric analysis without measurements of gas flow rates or mass spectrometer sensitivities. Scanning electron microprobe analysis, Mossbauer spectroscopy, and several other common analytical methods were also used. Calcined sludge consists primarily of amorphous particles of hydrous oxides with iron, manganese, nickel, and calcium distributed fairly uniformly throughout the powder. Iron, manganese, nickel, and calcium exist in forms that are highly insoluble in water, but aluminum, sulfate, nitrate, and sodium exhibit relative water solubilities that increase in the given order from 60% to 94%. Evolved gas analysis in a helium atmosphere showed that calcined sludge is completely dehydrated by heating to 400 0 C, carbon dioxide is evolved between 100 to 700 0 C with maximum evolution at 500 0 C, and oxygen is evolved between 400 and 1000 0 C. Evolved gas analyses are also reported for uncalcined sludge. A spinel-type oxide similar to NiFe 2 O 4 was detected by x-ray diffraction analysis at very low-level in calcined sludge

Microstructural changes in porous hematite nanoparticles upon calcination

DEFF Research Database (Denmark)

Johnsen, Rune; Knudsen, Kenneth D.; Molenbroek, Alfons M.

2011-01-01

This combined study using small-angle neutron scattering (SANS), X-ray powder diffraction (XRPD), transmission electron microscopy (TEM) and adsorption isotherm techniques demonstrates radical changes in the microstructure of porous hematite (-Fe2O3) nanoparticles upon calcination in air. TEM....... The change in microstructure also causes a reduction in the surface area as calculated by gaseous adsorption. The XRPD and SANS data show that the crystallite and SANS particle sizes are virtually unchanged by calcination at 623 K. Calcination at 973 K induces a significant alteration of the sample. The XRPD...... data reveal that the crystallite size increases significantly, and the SANS and adsorption isotherm studies suggest that the specific surface area decreases by a factor of 5–6. The TEM images show that the particles are sintered into larger agglomerates, but they also show that parts of the porous...

Voltammetric determination of zirconium using azo compounds

International Nuclear Information System (INIS)

Orshulyak, O.O.; Levitskaya, G.D.

2008-01-01

The optimum conditions for zirconium complexation with azo compounds are found. The applicability of Eriochrome Red B, Calcon, and Calcion to the voltammetric determination of zirconium, total Zr(IV) and Hf(IV), and Zr(IV) in the presence of Zn(II), Cu(II), Cd(II), Ni(II), or Ti(IV) is demonstrated. The developed procedures are used to determine zirconium in a terbium alloy and in an alloy for airplane wheel drums [ru

Calcination of Rod-like Hydroxyapatite Nanocrystals with an Anti-sintering Agent Surrounding the Crystals

International Nuclear Information System (INIS)

Okada, M.; Furuzono, T.

2007-01-01

Sintering-free nanocrystals of calcined hydroxyapatite (HAp) having a rod-like morphology were fabricated by calcination at 800 deg. C for 1 h with an anti-sintering agent surrounding original HAp particles and the agent was subsequently removed after calcination. The original HAp particles having a rod-like morphology with a size ranging from 30 to 80 nm (short axis) and 300 to 500 nm (long axis) were prepared by wet chemical process, and poly(acrylic acid, calcium salt) (PAA-Ca) was used as the anti-sintering agent. In the case of calcination without additives, the mean size of HAp crystals dispersed in an ethanol medium increased by about 4 times and the specific surface area of the crystals exhibited a 25% decrease compared to those of the original HAp particles because of calcination-induced sintering among the crystals. On the other hand, the HAp crystals calcined with the anti-sintering agent, PAA-Ca, could be dispersed in an ethanol medium at the same size as the original particles, and they preserved the specific surface area after calcination. These results indicate that PAA-Ca and/or its thermally decomposed product, CaO, surrounded the HAp particles and protected them against calcination-induced sintering during calcination. The HAp crystals calcined with PAA-Ca showed high crystallinity, and no other calcium phosphate phases could be detected after washing with water

URANIUM DECONTAMINATION WITH RESPECT TO ZIRCONIUM

Science.gov (United States)

Vogler, S.; Beederman, M.

1961-05-01

A process is given for separating uranium values from a nitric acid aqueous solution containing uranyl values, zirconium values and tetravalent plutonium values. The process comprises contacting said solution with a substantially water-immiscible liquid organic solvent containing alkyl phosphate, separating an organic extract phase containing the uranium, zirconium, and tetravalent plutonium values from an aqueous raffinate, contacting said organic extract phase with an aqueous solution 2M to 7M in nitric acid and also containing an oxalate ion-containing substance, and separating a uranium- containing organic raffinate from aqueous zirconium- and plutonium-containing extract phase.

ICPP calcined solids storage facility closure study. Volume III: Engineering design files

International Nuclear Information System (INIS)

1998-02-01

The following information was calculated to support cost estimates and radiation exposure calculations for closure activities at the Calcined Solids Storage Facility (CSSF). Within the estimate, volumes were calculated to determine the required amount of grout to be used during closure activities. The remaining calcine on the bin walls, supports, piping, and floor was also calculated to approximate the remaining residual calcine volumes at different stages of the removal process. The estimates for remaining calcine and vault void volume are higher than what would actually be experienced in the field, but are necessary for bounding purposes. The residual calcine in the bins may be higher than was is experienced in the field as it was assumed that the entire bin volume is full of calcine before removal activities commence. The vault void volumes are higher as the vault roof beam volumes were neglected. The estimations that follow should be considered rough order of magnitude, due to the time constraints as dictated by the project's scope of work. Should more accurate numbers be required, a new analysis would be necessary

ICPP calcined solids storage facility closure study. Volume III: Engineering design files

Energy Technology Data Exchange (ETDEWEB)

NONE

1998-02-01

The following information was calculated to support cost estimates and radiation exposure calculations for closure activities at the Calcined Solids Storage Facility (CSSF). Within the estimate, volumes were calculated to determine the required amount of grout to be used during closure activities. The remaining calcine on the bin walls, supports, piping, and floor was also calculated to approximate the remaining residual calcine volumes at different stages of the removal process. The estimates for remaining calcine and vault void volume are higher than what would actually be experienced in the field, but are necessary for bounding purposes. The residual calcine in the bins may be higher than was is experienced in the field as it was assumed that the entire bin volume is full of calcine before removal activities commence. The vault void volumes are higher as the vault roof beam volumes were neglected. The estimations that follow should be considered rough order of magnitude, due to the time constraints as dictated by the project`s scope of work. Should more accurate numbers be required, a new analysis would be necessary.

Effects of titanium and zirconium on iron aluminide weldments

Energy Technology Data Exchange (ETDEWEB)

Mulac, B.L.; Edwards, G.R. [Colorado School of Mines, Golden, CO (United States). Center for Welding, Joining, and Coatings Research; Burt, R.P. [Alumax Technical Center, Golden, CO (United States); David, S.A. [Oak Ridge National Lab., TN (United States). Metals and Ceramics Div.

1997-12-01

When gas-tungsten arc welded, iron aluminides form a coarse fusion zone microstructure which is susceptible to hydrogen embrittlement. Titanium inoculation effectively refined the fusion zone microstructure in iron aluminide weldments, but the inoculated weldments had a reduced fracture strength despite the presence of a finer microstructure. The weldments fractured by transgranular cleavage which nucleated at cracked second phase particles. With titanium inoculation, second phase particles in the fusion zone changed shape and also became more concentrated at the grain boundaries, which increased the particle spacing in the fusion zone. The observed decrease in fracture strength with titanium inoculation was attributed to increased spacing of second phase particles in the fusion zone. Current research has focused on the weldability of zirconium- and carbon-alloyed iron aluminides. Preliminary work performed at Oak Ridge National Laboratory has shown that zirconium and carbon additions affect the weldability of the alloy as well as the mechanical properties and fracture behavior of the weldments. A sigmajig hot cracking test apparatus has been constructed and tested at Colorado School of Mines. Preliminary characterization of hot cracking of three zirconium- and carbon-alloyed iron aluminides, each containing a different total concentration of zirconium at a constant zirconium/carbon ratio of ten, is in progress. Future testing will include low zirconium alloys at zirconium/carbon ratios of five and one, as well as high zirconium alloys (1.5 to 2.0 atomic percent) at zirconium/carbon ratios of ten to forty.

Production of nuclear grade zirconium: A review

Energy Technology Data Exchange (ETDEWEB)

Xu, L., E-mail: L.Xu-2@tudelft.nl [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110004 (China); Department of Materials Science and Engineering, Delft University of Technology, Delft 2628 CD (Netherlands); Xiao, Y. [Department of Metallurgical Engineering, Anhui University of Technology, Ma' anshan 243002 (China); Zr-Hf-Ti Metallurgie B.V., Den Haag 2582 SB (Netherlands); Sandwijk, A. van [Zr-Hf-Ti Metallurgie B.V., Den Haag 2582 SB (Netherlands); Xu, Q. [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110004 (China); Yang, Y. [Department of Materials Science and Engineering, Delft University of Technology, Delft 2628 CD (Netherlands)

2015-11-15

Zirconium is an ideal material for nuclear reactors due to its low absorption cross-section for thermal neutrons, whereas the typically contained hafnium with strong neutron-absorption is very harmful for zirconium as a fuel cladding material. This paper provides an overview of the processes for nuclear grade zirconium production with emphasis on the methods of Zr–Hf separation. The separation processes are roughly classified into hydro- and pyrometallurgical routes. The known pyrometallurgical Zr–Hf separation methods are discussed based on the following reaction features: redox characteristics, volatility, electrochemical properties and molten salt–metal equilibrium. In the present paper, the available Zr–Hf separation technologies are compared. The advantages and disadvantages as well as future directions of research and development for nuclear grade zirconium production are discussed.

Titanium(IV), zirconium, hafnium and thorium

International Nuclear Information System (INIS)

Brown, Paul L.; Ekberg, Christian

2016-01-01

Titanium can exist in solution in a number of oxidation states. The titanium(IV) exists in acidic solutions as the oxo-cation, TiO 2+ , rather than Ti 4+ . Zirconium is used in the ceramics industry and in nuclear industry as a cladding material in reactors where its reactivity towards hydrolysis reactions and precipitation of oxides may result in degradation of the cladding. In nature, hafnium is found together with zirconium and as a consequence of the contraction in ionic radii that occurs due to the 4f -electron shell, the ionic radius of hafnium is almost identical to that of zirconium. All isotopes of thorium are radioactive and, as a consequence of it being fertile, thorium is important in the nuclear fuel cycle. The polymeric hydrolysis species that have been reported for thorium are somewhat different to those identified for zirconium and hafnium, although thorium does form the Th 4 (OH) 8 8+ species.

Process Design Concepts for Stabilization of High Level Waste Calcine

Energy Technology Data Exchange (ETDEWEB)

T. R. Thomas; A. K. Herbst

2005-06-01

The current baseline assumption is that packaging ¡§as is¡¨ and direct disposal of high level waste (HLW) calcine in a Monitored Geologic Repository will be allowed. The fall back position is to develop a stabilized waste form for the HLW calcine, that will meet repository waste acceptance criteria currently in place, in case regulatory initiatives are unsuccessful. A decision between direct disposal or a stabilization alternative is anticipated by June 2006. The purposes of this Engineering Design File (EDF) are to provide a pre-conceptual design on three low temperature processes under development for stabilization of high level waste calcine (i.e., the grout, hydroceramic grout, and iron phosphate ceramic processes) and to support a down selection among the three candidates. The key assumptions for the pre-conceptual design assessment are that a) a waste treatment plant would operate over eight years for 200 days a year, b) a design processing rate of 3.67 m3/day or 4670 kg/day of HLW calcine would be needed, and c) the performance of waste form would remove the HLW calcine from the hazardous waste category, and d) the waste form loadings would range from about 21-25 wt% calcine. The conclusions of this EDF study are that: (a) To date, the grout formulation appears to be the best candidate stabilizer among the three being tested for HLW calcine and appears to be the easiest to mix, pour, and cure. (b) Only minor differences would exist between the process steps of the grout and hydroceramic grout stabilization processes. If temperature control of the mixer at about 80„aC is required, it would add a major level of complexity to the iron phosphate stabilization process. (c) It is too early in the development program to determine which stabilizer will produce the minimum amount of stabilized waste form for the entire HLW inventory, but the volume is assumed to be within the range of 12,250 to 14,470 m3. (d) The stacked vessel height of the hot process vessels

Mission Need Statement: Calcine Disposition Project Major Systems Acquisition Project

International Nuclear Information System (INIS)

J. T. Beck

2007-01-01

This document identifies the need to establish the Calcine Disposition Project to determine and implement the final disposition of calcine including characterization, retrieval, treatment (if necessary), packaging, loading, onsite interim storage pending shipment to a repository or interim storage facility, and disposition of related facilities

Recovery of gold and uranium from calcines

Energy Technology Data Exchange (ETDEWEB)

Livesey-Goldblatt, E.

1981-10-06

The invention concerns the recovery of non-ferrous metals, such as gold, uranium or the like from iron oxide containing calcines which have the non-ferrous metal present in solid solution and/or encapsulated within the iron oxide. The calcine is reacted, while stirring vigorously, with sulphuric acid or another strong inorganic acid to cause the iron to form the ferric salt. The material obtained is mixed with water and the liquid and solid phases are separated from each other. The non-ferrous metal is then obtained from at least one of these phases by leaching, or the like.

Translucency and Strength of High-Translucency Monolithic Zirconium-Oxide Materials

Science.gov (United States)

2016-05-12

Capt Todd D. Church APPROVED: Translucency and Strength of High-Translucency Monolithic Zirconium -Oxide Materials C~t) Kraig/[ Vandewalle Date...copyrighted material in the thesis/dissertation manuscript entitled: "Translucency arid Strength of High-Translucency Monolithic Zirconium -Oxide...Translucency Monolithic Zirconium -Oxide Materials Abstract Dental materials manufacturers have developed more translucent monolithic zirconium oxide

Review of zirconium-zircaloy pyrophoricity

International Nuclear Information System (INIS)

Cooper, T.D.

1984-11-01

Massive zirconium metal scrap can be handled, shipped, and stored with no evidence of combustion or pyrophoricity hazards. Mechanically produced fine scrap such as shavings, turnings, or powders can burn but are not pyrophoric unless the particle diameter is less than 54 μm. Powders with particle diameters less than 54 μm can be both pyrophoric and explosive. Pyrophoric powders should be collected and stored underwater or under inert gas cover to reduce the flammability hazard. Opening sealed containers of zirconium stored underwater should be attempted with caution since hydrogen may be present. The factors that influence the ignition temperature have been explored in depth and recommendations are included for the safe handling, shipping, and storage of pyrophoric or flammable zirconium. 29 refs., 5 figs., 6 tabs

Tests for depositing thin films of metallic zirconium; Essais de depot de zirconium metallique en couches minces

Energy Technology Data Exchange (ETDEWEB)

Bentolila, J.; Pattoret, A.; Platzer, R.

1957-01-15

The authors report a study which aimed at obtaining a thin, adhesive and non porous coating of metallic zirconium on a uranium substrate by means of chemical process. The main required condition was not to go beyond the uranium phase change temperature (650 C). Two kinds of tests have been performed: on the one hand, tests of reduction of zirconium tetrachloride in non aqueous solvent medium, and on the other hand, tests of vacuum decomposition of zirconium hydride. As far as the first tests are concerned, the authors studied organic solvent media (reduction by aluminium and lithium hydride, action of organic-magnesium compounds), and liquid ammoniac. For the second test type, they describe the apparatus, the preparation of the zirconium hydride, preparation of the substrate surfaces, coating preparation, and decomposition process. Results are discussed in terms of temperature, of presence of copper powder in the coating, of early surface hydriding of uranium, surface polishing.

Applied laboratory research of high-level waste denitration and calcination technologies

International Nuclear Information System (INIS)

Napravnik, J.

1977-01-01

Denitration and calcination processes are assessed for model solutions of high-level radioactive wastes. The kinetics was studied of the reaction of HNO 3 with HCOOH with respect to the final composition of the gaseous product. A survey is presented of used denitration agents and of reaction processes. Calcination was studied both as associated with denitration in a single technological step and separately. Also studied was the pyrolysis and chemical decomposition of sodium nitrate which forms an indecomposable melt in the temperature region of 320 to 850 degC under normal conditions. Based on the experiments a laboratory unit was designed and produced for the denitration and calcination of model solutions of high-level radioactive wastes operating in a temperature range of 100 to 550 degC with a capacity of 1000 ml/h. A boiler type stirred evaporator with electric heating (3 kW) was chosen for the denitration unit while a vertical calcinator modified from a film evaporator with a thermal input of 4 kW was chosen for the calcination unit. (B.S.)

RECONSTRUCTION OF CALCINED Zn -Al LAYERED DOUBLE HYDROXIDES DURING TETRACYCLINE ADSORPSION

Directory of Open Access Journals (Sweden)

G. M. Starukh

2015-12-01

Full Text Available Zn-Al mixed oxides containing ZnO different degree crystallinity were obtained by calcinations of Zn-Al layered double hydroxides (LDHs. The reconstruction of calcined Zn-Al LDHs has been performed under stirring in aqueous suspensions. The assynthesized LDHs, its decomposition products, as well as the reconstructed solids upon hydration were characterized by XRD, N2adsorption, differential and thermal gravimetric analysis. It was found that the ability of Zn-Al LDHs to recover a layered structure under the hydration of mixed oxides depends on the degree of ZnO crystallinity. The partial reconstruction of Zn-Al layered structure occurs in tetracycline solutions irrespective to the degree of ZnO crystallinity in calcined LDHs. Calcined Zn-Al LDHs demonstrate the higher adsorption capacity to tetracycline in comparison with as-prepared Zn-Al LDHs. The adsorption of TC on calcined and uncalcined ZnAl LDHs occurs on the centers of one particular type. It is suggested that surface complexation of the A-ring ligand of TC with Al-OH centers takes place.

Analysis of hafnium in zirconium alloys

International Nuclear Information System (INIS)

Kondo, Isao; Sakai, Fumiaki; Ohuchi, Yoshifusa; Nakamura, Hisashi

1977-01-01

It is required to analyse alloying components and impurity elements in the acceptance analysis of zirconium alloys as the material for fuel cladding tubes and pressure tubes for advanced thermal reactors. Because of extreme similarity in chemical properties between zirconium and hafnium, about 100 ppm of hafnium is usually contained in zirconium alloys. Zircaloy-2 alloy and 2.5% Nb-zirconium with the addition of hafnium had been prepared as in-house standard samples for rapid analysis. Study was made on fluorescent X-ray analysis and emission spectral analysis to establish the analytical method. By using these in-house standard samples, acceptance analysis was successfully carried out for the fuel cladding tubes for advanced thermal reactors. Sulfuric acid solution was prepared from JAERI-Z 1, 2 and 3, the standard sample for zircaloy-2 prepared by the Analytical Committee on Nuclear Fuel and Reactor Materials, JAERI, and zirconium oxide (Hf 1 ppm/Zr). Standard Hf solution was added to the sulfuric acid solution step by step, to make up a series of the standard oxide samples by the precipitation process. By the use of these standard samples, the development of the analytical method and joint analysis were made by the three-member analytical technique research group including PNC. The analytical precision for the fluorescent X-ray analysis was improved by attaching a metallic yttrium filter to the window of an X-ray tube so as to suppress the effect due to zirconium matrix. The variation factor of the joint analysis was about 10% to show good agreement, and the indication value was determined. (Kobatake, H.)

Letter report: Evaluation of dryer/calciner technologies for testing

International Nuclear Information System (INIS)

Sevigny, G.

1996-02-01

This letter report describes some past experiences on the drying and calcination of radioactive materials or corresponding simulants; and the information needed from testing. The report also includes an assessment of informational needs including possible impacts to a full-scale plant. This includes reliability, maintenance, and overall size versus throughput. Much of the material was previously compiled and reported by Mike Elliott of PNL open-quotes Melter Performance Assessmentclose quotes and Larry Eisenstatt of SEG on contract to WHC in a letter to Rod Powell. Also, an annotated bibliography was prepared by Reagan Seymour of WHC. Descriptions of the drying and calciner technologies, development status, advantages and disadvantages of using a WFE or calciner, and recommendations for future testing are discussed in this report

Removal of iron contaminant from zirconium chloride solution

International Nuclear Information System (INIS)

Voit, D.O.

1992-01-01

This patent describes a process for eliminating iron contaminant from an aqueous zirconium chloride solution that has been contaminated with FeCl 3 in a plant in which zirconium and hafnium chloride solutions are separated by a main MINK solvent extraction system and the FeCl 3 is normally removed from the zirconium chloride solution by a secondary MINK solvent extraction system

Dependency of Delayed Hydride Crack Velocity on the Direction of an Approach to Test Temperatures in Zirconium Alloys

International Nuclear Information System (INIS)

Kim, Young Suk; Kim, Kang Soo; Im, Kyung Soo; Ahn, Sang Bok; Cheong, Yong Moo

2005-01-01

Recently, Kim proposed a new DHC model where a driving force for the DHC is a supersaturated hydrogen concentration as a result of a hysteresis of the terminal solid solubility (TSS) of hydrogen in zirconium alloys upon a heating and a cooling. This model was demonstrated to be valid through a model experiment where the prior plastic deformation facilitated nucleation of the reoriented hydrides, thus reducing the supersaturated hydrogen concentration at the plastic zone ahead of the crack tip and causing hydrogen to move to the crack tip from the bulk region. Thus, an approach to the test temperature by a cooling is required to create a supersaturation of hydrogen, which is a driving force for the DHC of zirconium alloys. However, despite the absence of the supersaturation of hydrogen due to an approach to the test temperature by a heating, DHC is observed to occur in zirconium alloys at the test temperatures below 180 .deg. C. As to this DHC phenomenon, Kim proposed that stress-induced transformation from γ-hydrides to δ-hydrides is likely to be a cause of this, based on Root's observation that the γ-hydride is a stable phase at temperatures lower than 180 .deg. C. In other words, the hydrides formed at the crack tip would be δ-hydrides due to the stressinduced transformation while the bulk region still maintains the initial hydride phase or γ-hydrides. It should be noted that Ambler has also assumed the crack tip hydrides to be δ-hydrides. When the δ-hydrides or ZrH1.66 are precipitated at the crack tip due to the transformation of the γ-hydrides or ZrH, the crack tip will have a decreased concentration of dissolved hydrogen in zirconium, considering the atomic ratio of hydrogen and zirconium in the γ- and δ-hydrides. In contrast, due to no stress-induced transformation of hydrides, the bulk region maintains the initial concentration of dissolved hydrogen. Hence, there develops a difference in the hydrogen concentration or .C between the bulk and the

Dependency of Delayed Hydride Crack Velocity on the Direction of an Approach to Test Temperatures in Zirconium Alloys

Energy Technology Data Exchange (ETDEWEB)

Kim, Young Suk; Kim, Kang Soo; Im, Kyung Soo; Ahn, Sang Bok; Cheong, Yong Moo [Korea Atomic Energy Research Institute, Taejon (Korea, Republic of)

2005-07-01

Recently, Kim proposed a new DHC model where a driving force for the DHC is a supersaturated hydrogen concentration as a result of a hysteresis of the terminal solid solubility (TSS) of hydrogen in zirconium alloys upon a heating and a cooling. This model was demonstrated to be valid through a model experiment where the prior plastic deformation facilitated nucleation of the reoriented hydrides, thus reducing the supersaturated hydrogen concentration at the plastic zone ahead of the crack tip and causing hydrogen to move to the crack tip from the bulk region. Thus, an approach to the test temperature by a cooling is required to create a supersaturation of hydrogen, which is a driving force for the DHC of zirconium alloys. However, despite the absence of the supersaturation of hydrogen due to an approach to the test temperature by a heating, DHC is observed to occur in zirconium alloys at the test temperatures below 180 .deg. C. As to this DHC phenomenon, Kim proposed that stress-induced transformation from {gamma}-hydrides to {delta}-hydrides is likely to be a cause of this, based on Root's observation that the {gamma}-hydride is a stable phase at temperatures lower than 180 .deg. C. In other words, the hydrides formed at the crack tip would be {delta}-hydrides due to the stressinduced transformation while the bulk region still maintains the initial hydride phase or {gamma}-hydrides. It should be noted that Ambler has also assumed the crack tip hydrides to be {delta}-hydrides. When the {delta}-hydrides or ZrH1.66 are precipitated at the crack tip due to the transformation of the {gamma}-hydrides or ZrH, the crack tip will have a decreased concentration of dissolved hydrogen in zirconium, considering the atomic ratio of hydrogen and zirconium in the {gamma}- and {delta}-hydrides. In contrast, due to no stress-induced transformation of hydrides, the bulk region maintains the initial concentration of dissolved hydrogen. Hence, there develops a difference in the

High purity zirconium obtainment through the iodine compounds transport method

International Nuclear Information System (INIS)

Bolcich, J.C.; Zuzek, E.; Dutrus, S.M.; Corso, H.L.

1987-01-01

This paper describes the experimental method and the equipment designed, constructed and actually applied for the high purity zirconium obtainment from a zirconium sponge of the nuclear type. The mechanism of purification is based on the impure metal attack with gaseous iodine (at 200 deg C) to obtain zirconium tetra iodine as main product which is then transformed into a pure zirconium base (at 1000-1300 deg C), precipitating the metallic zirconium and releasing the gaseous iodine. From the first experiences carried out, pure zirconium has been obtained from an initial filament of 0.5 mm of diameter as well as wires up to 2.5 mm of diameter. This work presents the results from the studies and analysis made to characterize the material obtained. Finally, the refining methods to which the zirconium produced may be submitted so as to optimize the final purity are discussed. (Author)

Inductive classification of operating data from a fluidized bed calciner

International Nuclear Information System (INIS)

O'Brien, B.H.

1990-01-01

A process flowsheet expert system for a fluidized bed calciner which solidifies high-level radioactive liquid waste was developed from pilot-plant data using a commercial, inductive classification program. After initial classification of the data, the resulting rules were inspected and adjusted to match existing knowledge of process chemistry. The final expert system predicts performance of process flowsheets based upon the chemical composition of the calciner feed and has been successfully used to identify potential operational problems prior to calciner pilot-plant testing of new flowsheets and to provide starting parameters for pilot-plant tests. By using inductive classification techniques to develop the initial rules from the calciner pilot-plant data and using existing process knowledge to verify the accuracy of these rules, an effective expert system was developed with a minimum amount of effort. This method may be applied for developing expert systems for other processes where numerous operating data are available and only general process chemistry effects are known

Effects of Coke Calcination Level on Pore Structure in Carbon Anodes

Science.gov (United States)

Fang, Ning; Xue, Jilai; Lang, Guanghui; Bao, Chongai; Gao, Shoulei

2016-02-01

Effects of coke calcination levels on pore structure of carbon anodes have been investigated. Bench anodes were prepared by 3 types of cokes with 4 calcination temperatures (800°C, 900°C, 1000°C and 1100°C). The cokes and anodes were characterized using hydrostatic method, air permeability determination, mercury porosimetry, image analysis and confocal microscopy (CSLM). The cokes with different calcination levels are almost the same in LC values (19-20 Å) and real density (1.967-1.985 g/cm3), while the anode containing coke calcined at 900°C has the lowest open porosity and air permeability. Pore size distribution (represented by Anode H sample) can be roughly divided into two ranges: small and medium pores in diameter of 10-400 μm and large pores of 400-580 μm. For the anode containing coke calcined at 800°C, a number of long, narrow pores in the pore size range of 400-580 μm are presented among cokes particles. Formation of these elongated pores may be attributed to coke shrinkages during the anode baking process, which may develop cracking in the anode under cell operations. More small or medium rounded pores with pore size range of 10-400 μm emerge in the anodes with coke calcination temperatures of 900°C, 1000°C and 1100°C, which may be generated due to release of volatiles from the carbon anode during baking. For the anode containing coke calcined at 1100°C, it is found that many rounded pores often closely surround large coke particles, which have potential to form elongated, narrow pores.

Silicon-Polymer Encapsulation of High-Level Calcine Waste for Transportation or Disposal

International Nuclear Information System (INIS)

Loomis, G.G.; Miller, C.M.; Giansiracusa, J.A.; Kimmel, R.; Prewett, S.V.

2000-01-01

This report presents the results of an experimental study investigating the potential uses for silicon-polymer encapsulation of High Level Calcine Waste currently stored within the Idaho Nuclear Technology and Engineering Center (INTEC) at the Idaho National Engineering and Environmental Laboratory (INEEL). The study investigated two different applications of silicon polymer encapsulation. One application uses silicon polymer to produce a waste form suitable for disposal at a High Level Radioactive Waste Disposal Facility directly, and the other application encapsulates the calcine material for transportation to an offsite melter for further processing. A simulated waste material from INTEC, called pilot scale calcine, which contained hazardous materials but no radioactive isotopes was used for the study, which was performed at the University of Akron under special arrangement with Orbit Technologies, the originators of the silicon polymer process called Polymer Encapsulation Technology (PET). This document first discusses the PET process, followed by a presentation of past studies involving PET applications to waste problems. Next, the results of an experimental study are presented on encapsulation of the INTEC calcine waste as it applies to transportation or disposal of calcine waste. Results relating to long-term disposal include: (1) a characterization of the pilot calcine waste; (2) Toxicity Characteristic Leaching Procedure (TCLP) testing of an optimum mixture of pilot calcine, polysiloxane and special additives; and, (3) Material Characterization Center testing MCC-1P evaluation of the optimum waste form. Results relating to transportation of the calcine material for a mixture of maximum waste loading include: compressive strength testing, 10-m drop test, melt testing, and a Department of Transportation (DOT) oxidizer test

Quercetin as colorimetric reagent for determination of zirconium

Science.gov (United States)

Grimaldi, F.S.; White, C.E.

1953-01-01

Methods described in the literature for the determination of zirconium are generally designed for relatively large amounts of this element. A good procedure using colorimetric reagent for the determination of trace amounts is desirable. Quercetin has been found to yield a sensitive color reaction with zirconium suitable for the determination of from 0.1 to 50?? of zirconium dioxide. The procedure developed involves the separation of zirconium from interfering elements by precipitation with p-dimethylaminoazophenylarsonic acid prior to its estimation with quercetin. The quercetin reaction is carried out in 0.5N hydrochloric acid solution. Under the operating conditions it is indicated that quercetin forms a 2 to 1 complex with zirconium; however, a 2 to 1 and a 1 to 1 complex can coexist under special conditions. Approximate values for the equilibrium constants of the complexes are K1 = 0.33 ?? 10-5 and K2 = 1.3 ?? 10-9. Seven Bureau of Standards samples of glass sands and refractories were analyzed with excellent results. The method described should find considerable application in the analysis of minerals and other materials for macro as well as micro amounts of zirconium.

CALCIUM OXIDE CHARACTERISTICS PREPARED FROM AMBUNTEN’S CALCINED LIMESTONE

Directory of Open Access Journals (Sweden)

Fatimatul Munawaroh

2018-05-01

Full Text Available Calcium oxide (CaO and calcium carbonate (CaCO3 are widely used in industry. CaO and CaCO3 can be synthesized or derived from limestone. The purpose of this study to determine the characteristics of CaO calcined limestone from Ambunten Sumenep. Lime in calcined at 850 ° C for 6 hours. Characterization of X-ray fluorescence (XRF was conducted to determine the chemical composition of limestone, X-ray diffraction test (XRD to find the lime crystalline phase and FTIR test to determine the absorption of wave number. XRF test results showed that the limestone chemical composition consisted of Ca of 95.37% as the dominant element, Mg of 4.1%, Fe 0.17% and Y by 0.39%. The XRD test results showed that the limestone crystal phase is ankerite (Ca [Fe, Mg] [CO3] 2 and after the calcined phase calcination is vaterite (Ca [OH] 2, calcite (CaO and calcite (CaCO3. While the FTIR test results show that the CaO spectra are seen at 3741.24, 1417.12 and 874.14 cm-1.

Antimony removal from aqueous solutions using Zirconium hydroxide

International Nuclear Information System (INIS)

Petrescu, D.; Velciu, L.; Bucur, C.

2016-01-01

In this paper it is presented an experimental test for non-radioactive antimony removal from aqueous solutions using zirconium hydroxide powder. Also, it was studied how the temperature and pH influences antimony adsorption onto zirconium hydroxide surface. After the adsorption, solutions were filtered on Cellulose Mixed Ester Membrane with 0.2 μm pore size to remove the zirconium powder and then the aqueous solutions were sent to Inductively Coupled Plasma Optic Emission Spectrometry (ICP-OES) for quantitative analysis of Sb. Zirconium hydroxide powders were examined by optical microscopy. For the solutions that were tested at pH 4.5 and 10.2 the antimony concentration dropped below the detection limit of ICP-OES device, proof of antimony adsorption on zirconium hydroxide. Also, for the other tested solutions which had pH=12 the antimony concentration reduced with 77% and 80%. The temperature had no influence upon adsorption mechanism. (authors)

Development of a continuous process for adjusting nitrate, zirconium, and free hydrofluoric acid concentrations in zirconium fuel dissolver product

International Nuclear Information System (INIS)

Cresap, D.A.; Halverson, D.S.

1993-04-01

In the Fluorinel Dissolution Process (FDP) upgrade, excess hydrofluoric acid in the dissolver product must be complexed with aluminum nitrate (ANN) to eliminate corrosion concerns, adjusted with nitrate to facilitate extraction, and diluted with water to ensure solution stability. This is currently accomplished via batch processing in large vessels. However, to accommodate increases in projected throughput and reduce water production in a cost-effective manner, a semi-continuous system (In-line Complexing (ILC)) has been developed. The major conclusions drawn from tests demonstrating the feasibility of this concept are given in this report

LITERATURE REVIEW OF PUO2 CALCINATION TIME AND TEMPERATURE DATA FOR SPECIFIC SURFACE AREA

Energy Technology Data Exchange (ETDEWEB)

Daniel, G.

2012-03-06

The literature has been reviewed in December 2011 for calcination data of plutonium oxide (PuO{sub 2}) from plutonium oxalate Pu(C{sub 2}O{sub 4}){sub 2} precipitation with respect to the PuO{sub 2} specific surface area (SSA). A summary of the literature is presented for what are believed to be the dominant factors influencing SSA, the calcination temperature and time. The PuO{sub 2} from Pu(C{sub 2}O{sub 4}){sub 2} calcination data from this review has been regressed to better understand the influence of calcination temperature and time on SSA. Based on this literature review data set, calcination temperature has a bigger impact on SSA versus time. However, there is still some variance in this data set that may be reflecting differences in the plutonium oxalate preparation or different calcination techniques. It is evident from this review that additional calcination temperature and time data for PuO{sub 2} from Pu(C{sub 2}O{sub 4}){sub 2} needs to be collected and evaluated to better define the relationship. The existing data set has a lot of calcination times that are about 2 hours and therefore may be underestimating the impact of heating time on SSA. SRNL recommends that more calcination temperature and time data for PuO{sub 2} from Pu(C{sub 2}O{sub 4}){sub 2} be collected and this literature review data set be augmented to better refine the relationship between PuO{sub 2} SSA and its calcination parameters.

Molten salt extractive distillation process for zirconium-hafnium separation

International Nuclear Information System (INIS)

McLaughlin, D.F.; Stoltz, R.A.

1989-01-01

This patent describes an improvement in a process for zirconium-hafnium separation. It utilizes an extractive distillation column with a mixture of zirconium and hafnium tetrachlorides introduced into a distillation column having a top and bottom with hafnium enriched overheads taken from the top of the column and a molten salt solvent circulated through the column to provide a liquid phase, and with molten salt solvent containing zirconium chloride being taken from the bottom of the distillation column. The improvements comprising: utilizing a molten salt solvent consisting principally of lithium chloride and at least one of sodium, potassium, magnesium and calcium chlorides; stripping of the zirconium chloride taken from the bottom of the distillation column by electrochemically reducing zirconium from the molten salt solvent; and utilizing a pressurized reflux condenser on the top of the column to add the hafnium chloride enriched overheads to the molten salt solvent previously stripped of zirconium chloride

The influence of calcination on the physical and chemical properties of petroleum and mixed cokes

Energy Technology Data Exchange (ETDEWEB)

Sikora, K; Syrek, H

1980-01-01

Freshly prepared petroleum and coal-petroleum cokes, before utilization for the production of various materials, are subjected to calcining--thermal treatment in a neutral or reducing atmosphere without the admission of air at less than or equal to 1400/sup 0/. During calcining, stabilization of the physical and chemical properties of the cokes takes place. The properties of the obtained coke depend chiefly on the calcining time and temperature. During calcining, volatile substances are removed almost completely from the coke; the coke density is increased, and its structure is put in order; the electrical conductivity is improved; the mechanical strength is increased; and the reactivity of the coke is decreased. Laboratory studies were conducted on calcining mixed coal-petroleum cokes of two grades at 1200, 1250, and 1300/sup 0/ for 2-6 h. In the calcining products the content of volatile substances, the ash content, S content, and density were determined. It was ascertained that calcining of mixed coal-petroleum cokes goes analogously to calcining of pure petroleum cokes. Raising the temperature and increasing the time of calcining has a substantial effect on improvement of coke physical and chemical properties. For high-quality coke, calcining is to be carried out at greater than or equal to 1300/sup 0/ for 4-6 h, for ordinary coke at > 1200/sup 0/ and greater than or equal to 4 h. The results are regarded as starting data for an industrial study of the calcining process.

Stop Smoking—Tube-In-Tube Helical System for Flameless Calcination of Minerals

Directory of Open Access Journals (Sweden)

Nils Haneklaus

2017-11-01

Full Text Available Mineral calcination worldwide accounts for some 5–10% of all anthropogenic carbon dioxide (CO2 emissions per year. Roughly half of the CO2 released results from burning fossil fuels for heat generation, while the other half is a product of the calcination reaction itself. Traditionally, the fuel combustion process and the calcination reaction take place together to enhance heat transfer. Systems have been proposed that separate fuel combustion and calcination to allow for the sequestration of pure CO2 from the calcination reaction for later storage/use and capture of the combustion gases. This work presents a new tube-in-tube helical system for the calcination of minerals that can use different heat transfer fluids (HTFs, employed or foreseen in concentrated solar power (CSP plants. The system is labeled ‘flameless’ since the HTF can be heated by other means than burning fossil fuels. If CSP or high-temperature nuclear reactors are used, direct CO2 emissions can be divided in half. The technical feasibility of the system has been accessed with a brief parametric study here. The results suggest that the introduced system is technically feasible given the parameters (total heat transfer coefficients, mass- and volume flows, outer tube friction factors, and –Nusselt numbers that are examined. Further experimental work will be required to better understand the performance of the tube-in-tube helical system for the flameless calcination of minerals.

Techniques for chemical characterization of zirconium and its alloys

International Nuclear Information System (INIS)

Iyer, K.V.; Bassan, M.K.T.; Sudersanan, M.

2002-01-01

Chemical characterization of zirconium and its alloys such as zircaloy, Zr-Nb, etc for minor and trace constituents like Nb, Ti, Fe, Cr, Ni, Sn, Al etc has been carried out. Zirconium, being a major constituent, has been determined by gravimetry as zirconium oxide while other constituents like Nb, Ti, Fe have been determined by spectrophotometric methods. Other metals of importance at trace level have been estimated by AAS or ICPAES. The judicious use of both conventional and modern instrumental methods of analysis helps in the characterization of zirconium and its alloys for various major and minor constituents. The role of matrix effect in the determination was also investigated and methods have been worked out based on a preliminary separation of zirconium by a hydroxide precipitation. (author)

Proposed Atomic Energy of Canada Ltd. 99Mo waste calcination process

International Nuclear Information System (INIS)

Ramey, D.W.; Haas, P.A.; Malkemus, D.W.; McGinnis, C.P.; Meyers, E.S.; Patton, B.D.; Birdwell, J.F.; Jubin, R.T.; Coltharp, K.A.

1994-10-01

Atomic Energy of Canada Limited (AECL), at its Chalk River Laboratory, generates from 3000 to 5000 L/year of high-level fissile waste solution from the production of 99 Mo. In this Mo process, highly enriched uranium (93 wt % 235 U, total uranium basis) contained in uranium-aluminum alloy target rods is irradiated to produce the 99 Mo product. The targets are removed from the reactor and dissolved in a mercury nitrate-catalyzed reaction with nitric acid. The 99 Mo product is then recovered by passing the solution through an alumina (Al 2 O 3 ) column. During discussions with personnel from the Oak Ridge National Laboratory (ORNL) on September 10, 1992, the ORNL-developed technology formerly applied to the solidification of aqueous uranium waste (Consolidated Edison Uranium Solidification Program or CEUSP) was judged potentially applicable to the AECL 99 Mo waste. Under a Work-for-Others contract (no. ERD-92-1132), which began May 24, 1993, ORNL was tasked to determine the feasibility of applying the CEUSP (or a similar) calcination process to solidify AECL's 99 Mo waste for > 30 years of safe dry storage. This study was to provide sufficient detailed information on the applicability of a CEUSP-type waste solidification process to allow AECL to select the process which best suited its needs. As with the CEUSP process, evaporation of the waste and a simultaneously partial destruction of acid by reaction with formaldehyde followed by in situ waste can thermal denitration waste was chosen as the best means of solidification. Unlike the CEUSP material, the 99 Mo waste has a considerable number of problem volatile and semivolatile constituents which must be recovered in the off-gas treatment system. Mercury removal before calcination was seen as the best option

Intercalation chemistry of zirconium 4-sulfophenylphosphonate

International Nuclear Information System (INIS)

Svoboda, Jan; Zima, Vítězslav; Melánová, Klára; Beneš, Ludvík; Trchová, Miroslava

2013-01-01

Zirconium 4-sulfophenylphosphonate is a layered material which can be employed as a host for the intercalation reactions with basic molecules. A wide range of organic compounds were chosen to represent intercalation ability of zirconium 4-sulfophenylphosphonate. These were a series of alkylamines from methylamine to dodecylamine, 1,4-phenylenediamine, p-toluidine, 1,8-diaminonaphthalene, 1-aminopyrene, imidazole, pyridine, 4,4′-bipyridine, poly(ethylene imine), and a series of amino acids from glycine to 6-aminocaproic acid. The prepared compounds were characterized by powder X-ray diffraction, thermogravimetry analysis and IR spectroscopy and probable arrangement of the guest molecules in the interlayer space of the host is proposed based on the interlayer distance of the prepared intercalates and amount of the intercalated guest molecules. - Graphical abstract: Nitrogen-containing organic compounds can be intercalated into the interlayer space of zirconium 4-sulfophenylphosphonate. - Highlights: • Zirconium 4-sulfophenylphosphonate was examined as a host material in intercalation chemistry. • A wide range of nitrogen-containing organic compounds were intercalated. • Possible arrangement of the intercalated species is described

Chemistry of titanium, zirconium and thorium picramates

International Nuclear Information System (INIS)

Srivastava, R.S.; Agrawal, S.P.; Bhargava, H.N.

1976-01-01

Picramates of titanium, zirconium and thorium are prepared by treating the aqueous sulphate, chloride and nitrate solutions with sodium picramate. Micro-analysis, colorimetry and spectrophotometry are used to establish the compositions (metal : ligand ratio) of these picramates as 1 : 2 (for titanium and zirconium) and 1 : 4 (for thorium). IR studies indicate H 2 N → Me coordination (where Me denotes the metal). A number of explosive properties of these picramates point to the fact that the zirconium picramate is thermally more stable than the picramates of titanium and thorium. (orig.) [de

Thermochemistry of interaction between zirconium disulfate and sulfuric acid

International Nuclear Information System (INIS)

Dmitrieva, S.V.; Chekmarev, A.M.; Vorob'ev, A.F.

1988-01-01

Thermochemistry of Zr(SO 4 ) 2 x4H 2 O (1) interaction with water and sulfuric acid solutions of different concentrations is studied. It is established that the dependence of 1 solution enthalpy on acid concentration 1-bars of a complex polyextreme nature. It is noted that the increase in exothermic nature of dissolving during the increase of H 2 SO 4 concentration from 0.05 to 0.50 mol/l is explained by zirconium hydroxosulfate and fulfate complexes substitution for hydroxocomplexes. The endothermal nature of 1 interaction with concentrated (>3 mol/l) H 2 SO 4 solutions is conditioned by the formation of acidocomplexes. It is assumed that the abrupt growth of the exothermal nature of 1 interaction with sulfuric acid solutions with the concentration less than 0.05 mol/l with water is connected with colloid formation. 12 refs.; 2 figs

Influence of calcination temperature on the structure and morphology of HAp bioceramics

International Nuclear Information System (INIS)

Teixeira, C.M.L.; Santos, P.T.A.; Rodrigues, P.A.; Costa, A.C.F.M.

2012-01-01

This study aimed to evaluate the influence of calcination temperature on the structure and morphology of samples of hydroxyapatite (HAp) synthesized by the wet method. For hydroxyapatite was used as precursor solutions of calcium hydroxide and phosphoric acid 1M solution of calcium hydroxide was stirred and heated to 80 ° C and then dropwise with a solution of phosphoric acid. After the liquid was evaporated without an oven at 110 ° C and sieved. The sample of PA as synthesized was submitted to calcination at 900 °C and 1100 °C / 2 hours. The samples as synthesized and after calcination were characterized by XRD, XRF, FTIR, SEM. The XRD showed the presence of phase hydroxyapatite for samples without calcining and both calcination temperatures studied. FTIR spectra showed bands group and PO 4 3- , CO 3 2- . Through the SEM micrograph, there is the formation of agglomerates in the form of porous flakes approximately spherical shape. (author)

Test Plan for Radioactive Testing of a Vertical Direct Denitration Calciner

International Nuclear Information System (INIS)

COMPTON, J.A.

2000-01-01

Stored solutions containing plutonium and nitric acid and possibly uranium thorium and minor amounts of other substances will be used for development and demonstration of a vertical calciner direct denitration process for conversion of those to stable storable PuO 2 rich solids. Some of those solutions are quite dilute and very impure these require either pretreatment to make them suitable for calciner feed or an alternate stabilization method. Untreated scrap solutions containing some amounts of sulfate phosphate sodium and/or potassium may also be tested for suitability of direct denitration for conversion directly to PuO 2 -rich solids. A vertical calciner will be used to demonstrate the direct denitration process for converting plutonium-bearing liquors to stable plutonium-rich solids. The calciner and some of its ancillary equipment were previously tested with non-radioactive chemicals to demonstrate operability

Test Plan for Radioactive Testing of a Vertical Direct Denitration Calciner

International Nuclear Information System (INIS)

COMPTON, J.A.

2000-01-01

Stored solutions containing plutonium and nitric acid and possibly uranium thorium and minor amounts of other substances will be used for development and demonstration of a vertical calciner direct denitration process for conversion of those to stable storable PuO 2 rich solids. Some of those solutions are quite dilute and very impure these require either pretreatment to make them suitable for calciner feed or an alternate stabilization method. Untreated scrap solutions containing some amounts of sulfate phosphate sodium and/or potassium may also be tested for suitability of direct denitration for conversion directly to PuO 2 -rich solids. A vertical calciner will be used to demonstrate the direct denitration process for converting plutonium-bearing liquors to stable plutonium rich solids. The calciner and some of its associated equipment were previously tested with non-radioactive chemicals to demonstrate operability

Test Plan for Radioactive Testing of a Vertical Direct Denitration Calciner

Energy Technology Data Exchange (ETDEWEB)

COMPTON, J.A.

2000-02-03

Stored solutions containing plutonium and nitric acid and possibly uranium thorium and minor amounts of other substances will be used for development and demonstration of a vertical calciner direct denitration process for conversion of those to stable storable PuO{sub 2} rich solids. Some of those solutions are quite dilute and very impure these require either pretreatment to make them suitable for calciner feed or an alternate stabilization method. Untreated scrap solutions containing some amounts of sulfate phosphate sodium and/or potassium may also be tested for suitability of direct denitration for conversion directly to PuO{sub 2}-rich solids. A vertical calciner will be used to demonstrate the direct denitration process for converting plutonium-bearing liquors to stable plutonium-rich solids. The calciner and some of its ancillary equipment were previously tested with non-radioactive chemicals to demonstrate operability.

Test Plan for Radioactive Testing of a Vertical Direct Denitration Calciner

Energy Technology Data Exchange (ETDEWEB)

COMPTON, J.A.

2000-02-03

Stored solutions containing plutonium and nitric acid and possibly uranium thorium and minor amounts of other substances will be used for development and demonstration of a vertical calciner direct denitration process for conversion of those to stable storable PuO{sub 2} rich solids. Some of those solutions are quite dilute and very impure these require either pretreatment to make them suitable for calciner feed or an alternate stabilization method. Untreated scrap solutions containing some amounts of sulfate phosphate sodium and/or potassium may also be tested for suitability of direct denitration for conversion directly to PuO{sub 2}-rich solids. A vertical calciner will be used to demonstrate the direct denitration process for converting plutonium-bearing liquors to stable plutonium rich solids. The calciner and some of its associated equipment were previously tested with non-radioactive chemicals to demonstrate operability.

Storage and characterization of the hydrogen in mixed oxides on base of cerium-nickel and zirconium or the aluminium

International Nuclear Information System (INIS)

Debeusscher, S.

2008-12-01

The mixed oxides based on cerium-nickel and zirconium or aluminium are able to store large quantities of hydrogen, To determine nature, reactivity and properties of hydrogen species (spill-over, direct desorption), the solid were studied by different physicochemical techniques in the dried, calcined and partially reduced states: XRD, porosity, TGA, TPR, TPA, TPD, chemical titration and inelastic neutron scattering (INS). Solids are mainly meso-porous with a common pore size at 4 nm, They are constituted of CeO 2 phase, Ce-Ni or Ce-Ni-Zr solid solution and of Ni(OH) 2 in the dried state and NiO in the calcined state. The Ni species are in various environments and the strong interactions between the cations in solid solution and at different particles interface influence their reducibility and the creation of anionic vacancies. Activation in H 2 in temperature is determining for hydrogen storage in the solid while calcination step is not necessary. INS Analyses evidence that the hydrogen species inserted during treatment in H 2 are H + (OH - ), hydride H - and H * (metallic nickel) species, present in various chemical environments, in particular for hydride species. All kinds of hydrogen species participate to the reaction during the chemical titration in agreement with the proposed hydrogenation mechanism. The study of the adsorption of hydrogen shows that this step is fast and in quantity of the same order as that measured by chemical titration. The direct desorption of H 2 is very low, linked to the presence of hydrogen in interaction with metallic nickel (H *- .). Desorption of water is also observed, in parallel, corresponding to the elimination of groups. The hydride species are not desorbed. These various observations allow connecting hydrogen species properties with their localization in the structure and to model active sites. (author)

Activity Based Startup Plan for Prototype Vertical Denitration Calciner

International Nuclear Information System (INIS)

SUTTER, C.S.

1999-01-01

Testing activation on the Prototype Vertical Denitration Calciner at PFP were suspended in January 1997 due to the hold on fissile material handling in the facility. The restart of testing activities will require a review through an activity based startup process based upon Integrated Safety Management (ISM) principles to verify readiness. The Activity Based Startup Plan for the Prototype vertical Denitration Calciner has been developed for this process

Remotely replaceable fuel and feed nozzles for the NWCF calciner vessel

International Nuclear Information System (INIS)

Fletcher, R.D.; Carter, J.A.; May, K.W.

1978-01-01

The development and testing of remotely replaceable fuel and feed nozzles for calcination of liquid radioactive wastes in the calciner vessel of the New Waste Calcining Facility (NWCF) being built at the Idaho National Engineering Laboratory are described. A complete fuel nozzle assembly was fabricated and tested at the Remote Maintenance Development Facility to evolve design refinements, identify required support equipment, and develop handling techniques. The design also provided for remote replacement of the nozzle support carriage and adjacent feed and fuel pipe loops using two pairs of master-slave manipulators

21 CFR 700.16 - Use of aerosol cosmetic products containing zirconium.

Science.gov (United States)

2010-04-01

... zirconium. 700.16 Section 700.16 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN... cosmetic products containing zirconium. (a) Zirconium-containing complexes have been used as an ingredient... indicates that certain zirconium compounds have caused human skin granulomas and toxic effects in the lungs...

Zirconium alloy fuel cladding resistant to PCI crack propagation

International Nuclear Information System (INIS)

Boyle, R.F.; Foster, J.P.

1987-01-01

A nuclear fuel element is described cladding tube comprising: concentric tubular layers of zirconium base alloys; the concentric tubular layers including an inner layer and outer layer; the outer layer metallurgically bonded to the inner layer; the outer layer composed of a first zirconium base alloy characterized by excellent resistance to corrosion caused by exposure to high temperature and pressure aqueous environments; the inner layer composed of a second zirconium base alloy consisting of: about 0.2 to 0.6 wt.% tin, about 0.03 to 0.11 wt.% iron, less than about 0.02 wt.% chromium, up to about 350 ppm oxygen and the remainder being zirconium and incidental impurities, and the inner layer characterized by improved resistance to crack propagation under reactor operating conditions compared to the first zirconium alloy

Test Plan for Radioactive Testing of a Vertical Direct Denitration Calciner

International Nuclear Information System (INIS)

COMPTON, J.A.

1999-01-01

A vertical calciner will be used to demonstrate the direct denitration process for converting plutonium-bearing liquors to stable plutonium rich solids. The calciner and some of its associated equipment were previously tested with non-radioactive chemicals to demonstrate operability

Test Plan for Radioactive Testing of a Vertical Direct Denitration Calciner

Energy Technology Data Exchange (ETDEWEB)

COMPTON, J.A.

1999-10-05

A vertical calciner will be used to demonstrate the direct denitration process for converting plutonium-bearing liquors to stable plutonium rich solids. The calciner and some of its associated equipment were previously tested with non-radioactive chemicals to demonstrate operability.

Waterside corrosion of zirconium alloys in nuclear power plants

International Nuclear Information System (INIS)

1998-01-01

Technically the study of corrosion of zirconium alloys in nuclear power reactors is a very active field and both experimental work and understanding of the mechanisms involved are going through rapid changes. As a result, the lifetime of any publication in this area is short. Because of this it has been decided to revise IAEA-TECDOC-684 - Corrosion of Zirconium Alloys in Nuclear Power Plants - published in 1993. This updated, revised and enlarged version includes major changes to incorporate some of the comments received about the first version. Since this review deals exclusively with the corrosion of zirconium and zirconium based alloys in water, and another separate publication is planned to deal with the fuel-side corrosion of zirconium based fuel cladding alloys, i.e. stress corrosion cracking, it was decided to change the original title to Waterside Corrosion of Zirconium Alloys in Nuclear Power Plants. The rapid changes in the field have again necessitated a cut-off date for incorporating new data. This edition incorporates data up to the end of 1995; including results presented at the 11 International Symposium on Zirconium in the Nuclear Industry held in Garmisch-Partenkirchen, Germany, in September 1995. The revised format of the review now includes: Introductory chapters on basic zirconium metallurgy and oxidation theory; A revised chapter discussing the present extent of our knowledge of the corrosion mechanism based on laboratory experiments; a separate and revised chapter discussing hydrogen uptake; a completely reorganized chapter summarizing the phenomenological observations of zirconium alloy corrosion in reactors; a new chapter on modelling in-reactor corrosion; a revised chapter devoted exclusively to the manner in which irradiation might influence the corrosion process; finally, a summary of our present understanding of the corrosion mechanisms operating in reactor

Hot zirconium cathode sputtered layers for useful surface modification

International Nuclear Information System (INIS)

Duckworth, R.G.

1986-01-01

It has been found that multilayer zirconium based sputtered coatings can greatly improve the wear properties of a wide variety of mechanical components, machine tools, and metal surfaces. Although a hot (approximately 1000 0 C) cathode is employed, temperature sensitive components can be beneficially treated, and for precision parts a total coating thickness of only 0.5μm is often perfectly effective. Even at the highest coating rates substrate temperatures are below 300 0 C. For the corrosion protection of less well finished surfaces thicker layers are usually required and it is important that relatively stress free layers are produced. The authors employed a variety of tailored zirconium/zirconium nitride/zirconium oxide mixed layers to solve a number of tribological problems for some 5 or 6 years. However, it is only recently that they designed, built, and commissioned rapid cycle, multiple cathode, load-lock plant for economic production of such coatings. This paper provides an introduction to this method of depositing pure zirconium and pure synthetic zirconium nitride films

Determination of microquantities of zirconium and thorium in uranium dioxide

International Nuclear Information System (INIS)

Weber de D'Alessio, Ana; Zucal, Raquel.

1975-07-01

A method for the determination of 10 to 50 ppm of zirconium and thorium in uranium IV oxide of nuclear purity is established. Zirconium and thorium are retained in a strong cation-exchange resin Dowex 50 WX8 in 1 M HCl. Zirconium is eluted with 0,5% oxalic acid solution and thorium with 4% ammonium oxalate. The colorimetric determination of zirconium with xilenol orange is done in perchloric acid after destructtion of oxalic acid and thorium is determined with arsenazo III in 5 M HCl. 10 μg of each element were determined with a standard deviation of 2,1% for thorium and 3,4% for zirconium. (author) [es

Calcining natural zeolites to improve their effect on cementitious mixture workability

International Nuclear Information System (INIS)

Seraj, Saamiya; Ferron, Raissa D.; Juenger, Maria C.G.

2016-01-01

Despite the benefits to long-term concrete durability, the use of natural zeolites as supplementary cementitious materials (SCMs) is uncommon due to their high water demand. The motivation of the research presented here was to better understand how the physical and chemical characteristics of natural zeolites influenced the workability of cementitious mixtures and whether those properties could be modified through calcination to mitigate the high water demand of natural zeolites. In this research, three different natural zeolites were characterized in their original and calcined states using x-ray diffraction (XRD) and Brunauer–Emmett–Teller (BET) surface area measurements. Rheology experiments were then conducted on cementitious pastes containing these natural zeolites, in their original and calcined states, to assess mixture viscosity and yield stress. Results showed that calcination destabilized the structure of the natural zeolites and reduced their surface area, which led to an improvement in mixture viscosity and yield stress.

Analysis of hydrogen in zirconium metallic

International Nuclear Information System (INIS)

Rodrigues, A.N.; Vega Bustillos, J.O.W.

1991-02-01

Determination of hydrogen in zirconium metallic have been performed using the hot vacuum extraction system and the gas chromatographic technique. The zirconium metallic samples were hydrieded by electrolitic technique at difference temperatures and times, then the samples were annealing at vacuum and eatching by fluoridric acid solution. The details of the hydrieded process, analytical technique and the data obtained are discussed. (author)

Development of zirconium hydride highly effective moderator materials

International Nuclear Information System (INIS)

Yin Changgeng

2005-10-01

The zirconium hydride with highly content of hydrogen and low density is new efficient moderator material for space nuclear power reactor. Russia has researched it to use as new highly moderator and radiation protection materials. Japanese has located it between the top of pressure vessel and the main protection as a shelter, the work temperature is rach to 220 degree C. The zirconium hydride moderator blocks are main parts of space nuclear power reactor. Development of zirconium hydride moderator materials have strength research and apply value. Nuclear Power Research and Design Instituteoh China (NPIC) has sep up the hydrogenation device and inspect systems, and accumurate a large of experience about zirconium hydride, also set up a strict system of QA and QC. (authors)

Separation process of zirconium and hafnium; Procede de separation du zirconium et du hafnium

Energy Technology Data Exchange (ETDEWEB)

Hure, J; Saint-James, R [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

1955-07-01

About the separation different processes of zirconium-hafnium, the extraction by solvent in cross-current is the most easily the process usable on an industrial scale. It uses tributyl phosphate as solvent, diluted with white spirit to facilitate the decanting. Some exploratory tests showed that nitric environment seemed the most favorable for extraction; but a lot of other factors intervene in the separation process. We studied the influence of the acidity successively, the NO{sub 3}{sup -} ions concentration, the role of the cation coming with NO{sub 3}{sup -}, as well as the influence of the concentration of zirconium in the solution on the separation coefficient {beta} = {alpha}{sub Zr} / {alpha}{sub Hf}. (M.B.) [French] Des differents procedes de separation zirconium-hafnium, l'extraction par solvant en contre-courant est le procede le plus facilement utilisable a l'echelle industrielle. On utilise comme solvant le phosphate de tributyle, dilue avec du white spirit pour faciliter les decantations. Des essais preliminaires ont montre que le milieu nitrique semblait le plus favorable a l'extraction; mais beaucoup d'autres facteurs interviennent dans le processus de separation. Nous avons etudie successivement l'influence de l'acidite, celle de la concentration en ions NO{sub 3}{sup -}, le role du cation accompagnant NO{sub 3}{sup -}, ainsi que l'influence de la concentration en zirconium de la solution sur le coefficient de separation {beta} = {alpha}{sub Zr} / {alpha}{sub Hf}. (MB)

Model of fragmentation of limestone particles during thermal shock and calcination in fluidised beds

Energy Technology Data Exchange (ETDEWEB)

Saastamoinen, J.; Pikkarainen, T.; Tourunen, A.; Rasanen, M.; Jantti, T. [VTT Technical Research Center, Jyvaskyla (Finland)

2008-11-15

Fragmentation of limestone due to thermal shock and calcination in a fluidised bed was studied through experiments and modelling. The time for heating was estimated by model calculations and the time for calcination by measurements. Fragmentation due to thermal shock was carried out by experiments in a CO{sub 2} atmosphere in order to prevent the effect of calcination. It was found to be much less than fragmentation due to calcination. Average particle sizes before and after fragmentation are presented for several types of limestone. The effects of particle size and gas composition on the primary fragmentation were studied through experiments. Increasing the fluidisation velocity increased the tendency to fragment. The evolution of the particle size distribution (PSD) of limestone particles due to thermal shock and during calcination (or simultaneous calcination and sulphation) were calculated using a population balance model. Fragmentation due to thermal shock is treated as an instantaneous process. The fragmentation frequency during calcination is presented as exponentially decaying over time. In addition to the final PSD, this model also predicts the PSD during the calcination process. The fragmentation was practically found to end after 10 min. Furthermore. a population balance method to calculate the particle size distribution and amount of limestone in fluidised beds in dynamic and steady state, when feeding history is known, is presented.

Design and performance of a full-scale spray calciner for nonradioactive high-level-waste-vitrification studies

International Nuclear Information System (INIS)

Miller, F.A.

1981-06-01

In the spray calcination process, liquid waste is spray-dried in a heated-wall spray dryer (termed a spray calciner), and then it may be combined in solid form with a glass-forming frit. This mixture is then melted in a continuous ceramic melter or in an in-can melter. Several sizes of spray calciners have been tested at PNL- laboratory scale, pilot scale and full scale. Summarized here is the experience gained during the operation of PNL's full-scale spray calciner, which has solidified approx. 38,000 L of simulated acid wastes and approx. 352,000 L of simulated neutralized wastes in 1830 h of processing time. Operating principles, operating experience, design aspects, and system descriptions of a full-scale spray calciner are discussed. Individual test run summaries are given in Appendix A. Appendices B and C are studies made by Bechtel Inc., under contract by PNL. These studies concern, respectively, feed systems for the spray calciner process and a spray calciner vibration analysis. Appendix D is a detailed structural analysis made at PNL of the spray calciner. These appendices are included in the report to provide a complete description of the spray calciner and to include all major studies made concerning PNL's full-scale spray calciner

Redox calcination study of Synroc D powder containing simulated SRL waste

International Nuclear Information System (INIS)

Chen, C.

1982-01-01

According to Ringwood [A.E. Ringwood, W. Sinclair, and G.M. McLaughlin, Nuclear Waste Immobilization, Lawrence Livermore Laboratory, Livermore, Rept. UCRL-15147 (1979)], the iron oxidation state is important in controlling, the spinel mineralogy and composition if the amount of titania (TiO 2 ) consumed in spinel formation is to be minimized in favor of the formation of the Synroc phases, zirconolite, perovskite, and nepheline. In our redox calcination studies we observed that the iron oxidation state of FeO/Fe 2 O 3 can be controlled by the redoxcalcining atmosphere. In a CO atmosphere, the oxidation state was reduced to less than 7 wt % Fe 2 O 3 . With appropriate CO 2 /CO gas mixtures the resultant iron oxidation states were in the range of 45 to 59 wt % Fe 2 O 3 . Direct rotary redox calcination of spray dried powder at 600 0 C, without prior air calcination, showed increased redox efficiency when compared to powder that had been previously air calcined at 650 0 C. We believe this is caused by a reduction in particle size. Rotary calcination at 800 0 C in argon has no measurable reduction affect on the iron oxidation state of Synroc D powder

A study of the fixing of phosphoric ions by zirconium-montmorillonite; Etude de la fixation d'ions phosphoriques par la montmorillonite-zirconium

Energy Technology Data Exchange (ETDEWEB)

Bittel, R; Boursat, C; Platzer, R [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

1960-07-01

In connection with the research carried out on the purification of nuclear reactor water, we have undertaken a study of the ion-exchange properties of acid montmorillonite. In a previous paper, we described the preparation of zirconium-montmorillonite small plate. The present article aims to study some of the properties of the clay obtained. We have observed that zirconium-montmorillonite fixes very strongly the phosphorus from solutions of phosphoric acid or of phosphates: on 1 g of clay it is possible to fix 1,2 milli-atoms-gram of zirconium and the zirconium montmorillonite itself fixes 2,1 milli-atoms-gram of phosphorus. An explanation of these experimental results, which is as much chemical as mineralogical, is the hypothesis that the fixing of phosphoric ions modifies the distribution of the ions between the platelets and precipitates a very slightly soluble product of the type diphospho-zirconic acid. (author) [French] En rapport avec des recherches sur I'epuration de l'eau des reacteurs nucleaires nous avons entrepris une etude sur les proprietes d'echangeur d'ions de la montmorillonite-acide. Dans une precedente publication, nous avons decrit la preparation des plaquettes de montmorillonite-zirconium. La presente communication a pour but d'etudier quelques proprietes de l'argile obtenue. Nous avons constate que la montmorilionite-zirconium fixe le phosphore de solutions d'acide phosphorique ou de phosphate avec une grande intensite: sur 1 g d'argile, on peut fixer 1,2 atomes-gramme de zirconium, et la montmorillonite-zirconium fixe a son tour 2,1 milli-atomesgramme de phosphore. Une explication des resultats experimentaux, tant d'ordre chimique que d'ordre mineralogique, consiste en l'hypothese suivant laquelle la fixation d'ions phosphoriques modifierait la repartition des ions entre les feuillets avec precipitation du compose tres peu soluble (type: acide diphosphozirconique). (auteur)

Sodium zirconium phosphate (NZP) as a host structure for nuclear waste immobilization: A review

International Nuclear Information System (INIS)

Scheetz, B.E.; Agrawal, D.K.; Breval, E.; Roy, R.

1994-01-01

Sodium zirconium phosphate [NZP] structural family, of which NaZr 2 P 3 O 12 is the parent composition, has been reviewed as a host ceramic waste form for nuclear waste immobilization. NZP compounds are characterized for their ionic conductivity, low thermal expansion and structural flexibility to accommodate a large number of multivalent ions. This latter property of the [NZP] structure allows the incorporation of almost all 42 nuclides present in a typical commercial nuclear waste. The leach studies of simulated waste forms based on NZP have shown reasonable resistance for the release of its constituents. The calculation of dissolution rates of NZP structure has demonstrated that it would take 20,000 times longer to dissolved NZP than quartz

A computation model for the corrosion resistance of nanocrystalline zirconium metal

International Nuclear Information System (INIS)

Zhang Xiyan; Shi Minghua; Liu Nianfu; Wei Yiming; Li Cong; Qiu Shaoyu; Zhang Qiang; Zhang Pengcheng

2007-01-01

In this paper a computation model of corrosion rate-grain size of nanocrystalline and ultra-fine zirconium has been presented. The model is based on the Wagner's theory and the electron theory of solids. The conductivity, electronic mean free path and grain size of metal were considered. By this model, the corrosion rate of zirconium metal under different temperature was computed. The results show that the corrosion weight gain and rate constant of nanocrystalline zirconium is lower than that of zirconium with coarse grain size. And the corrosion rate constant and weight gain of nanocrystalline zirconium metal decrease with the decrease of grain size. So the refinement of grain size can remarkably improve the corrosion resistance of zirconium metal. (authors)

40 CFR 721.10089 - Modified salicylic acid, zirconium complex (generic).

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Modified salicylic acid, zirconium... Specific Chemical Substances § 721.10089 Modified salicylic acid, zirconium complex (generic). (a) Chemical... as modified salicylic acid, zirconium complex (PMN P-00-552) is subject to reporting under this...

Preparation of complexes of zirconium and hafnium tetrachlorides with phosphorus oxychloride

International Nuclear Information System (INIS)

McLaughlin, D.F.

1989-01-01

This patent describes an improvement in a method for separating hafnium tetrachloride from zirconium tetrachloride where a complex of zirconium-hafnium tetrachlorides and phosphorus oxychloride is prepared from zirconium-hafnium tetrachlorides and the complex of zirconium-hafnium tetrachlorides and phosphorus oxychloride is introduced into a distillation column, which distillation column has a reboiler connected at the bottom and a reflux condenser connected at the top and where a hafnium tetrachloride enriched stream is taken from the top of the column and a zirconium enriched tetrachloride stream is taken from the bottom of the column. The improvement comprising: prepurifying the zirconium-hafnium tetrachlorides, prior to preparation of the complex and introduction of the complex into a distillation column, to substantially eliminate iron chloride from the zirconium hafnium tetrachlorides, whereby buildup or iron chloride in the distillation column and in the reboiler is substantially eliminated and the column can be operated in a continuous, stable and efficient manner

Low cycle fatigue behaviour of zirconium alloys at 3000C

International Nuclear Information System (INIS)

Hosbons, R.R.

1975-01-01

The low cycle fatigue lives of two zirconium alloys, zirconium--2.5 wt percent niobium and zirconium--1.1 wt percent chromium--0.1 wt percent iron, have been determined at 300 0 C. Both annealed material and cold-worked and stress-relieved material have similar fatigue lives to annealed Zircaloy-2 but β-quenched zirconium--niobium and zirconium--chromium--iron have lower fatigue lives than annealed Zircaloy-2. An atmosphere containing a concentration of iodine lower than that required for stress corrosion cracking still significantly lowers the fatigue life. A mathematical relationship between fatigue life and short-term tensile properties was used to estimate the fatigue life of zirconium alloy fuel sheaths and it was estimated that for a strain cycle of 0.1 percent a cyclic frequency exceeding 0.116 Hz (10,000 cycles/ day) would be required to cause fatigue failure of the sheath before its design life is realized

Low cycle fatigue behaviour of zirconium alloys at 3000C

International Nuclear Information System (INIS)

Hosbons, R.R.

1975-01-01

The low cycle fatigue lives of two zirconium alloys, zirconium-2.5 wt% niobium and zirconium-1.1 wt% chronium-0.1 wt% iron, have been determined at 300 0 C. Both annealed material and cold-worked and stress-relieved material have similar fatigue lives to annealed Zircaloy-2 but β-quenched zirconium-niobium and zirconium-chromium-iron have lower fatigue lives than annealed Zircaloy-2. An atmosphere containing a concentration of iodine lower than that required for stress corrosion cracking still significantly lowers the fatigue life. A mathematical relationship between fatigue life and short-term tensile properties was used to estimate the fatigue life of zirconium alloy fuel sheaths and it was estimated that for a strain cycle of 0.1 per cent a cyclic frequency exceeding 0.116 Hz (10 000 cycles/day) would be required to cause fatigue failure of the sheath before its design life is realized. (author)

Investigation of anodic oxide coatings on zirconium after heat treatment

International Nuclear Information System (INIS)

Sowa, Maciej; Dercz, Grzegorz; Suchanek, Katarzyna; Simka, Wojciech

2015-01-01

Highlights: • Oxide layers prepared via PEO of zirconium were subjected to heat treatment. • Surface characteristics were determined for the obtained oxide coatings. • Heat treatment led to the partial destruction of the anodic oxide layer. • Pitting corrosion resistance of zirconium was improved after the modification. - Abstract: Herein, results of heat treatment of zirconium anodised under plasma electrolytic oxidation (PEO) conditions at 500–800 °C are presented. The obtained oxide films were investigated by means of SEM, XRD and Raman spectroscopy. The corrosion resistance of the zirconium specimens was evaluated in Ringer's solution. A bilayer oxide coatings generated in the course of PEO of zirconium were not observed after the heat treatment. The resulting oxide layers contained a new sublayer located at the metal/oxide interface is suggested to originate from the thermal oxidation of zirconium. The corrosion resistance of the anodised metal was improved after the heat treatment

Calcination of calcium acetate and calcium magnesium acetate: effect of the reacting atmosphere

Energy Technology Data Exchange (ETDEWEB)

Adanez, J.; Diego, L.F. de; Garcia-Labiano, F. [Instituto de Carboquimica, Zaragoza (Spain). Dept. of Energy and Environment

1999-04-01

The calcination process of the calcium acetate (CA) and calcium magnesium acetate (CMA) was investigated as a previous step for coal gas desulfurisation during sorbent injection at high temperatures because the excellent results demonstrated by these sorbents as sulfur removal agents both in combustion and gasification processes. As pore structure developed during calcination is one of the most important characteristics of the sorbent related with the later reaction with the gaseous pollutants, several calcination tests were conducted in a drop tube reactor at temperatures from 700{degree}C to 1100{degree}C, and residence times from 0.8 to 2.4 s. Four different gas atmospheres were used for comparative purposes: inert, oxidising, reducing, and non-calcining (pure CO{sub 2}). Despite the advantage of the high porous cenospheric structure developed by these sorbents during their injection at high temperature, calcination of the CaCO{sub 3} was not complete even at the longest residence time, 2.4 s, and the highest temperature, 1100{degree}C, tested. An important effect of the reacting atmosphere on the calcination conversion and on the sorbent pore structure was detected. The CO{sub 2} concentration around the particle, both that fed in the reacting gases or that generated by organic material combustion, seems to be responsible for the final calcination conversions obtained in each case, also affecting the sintering suffered by the sorbents. 19 refs., 10 figs.

New Waste Calcining Facility (NWCF) Waste Streams

International Nuclear Information System (INIS)

K. E. Archibald

1999-01-01

This report addresses the issues of conducting debris treatment in the New Waste Calcine Facility (NWCF) decontamination area and the methods currently being used to decontaminate material at the NWCF

Experimental study on the effect of calcination on the volcanic ash activity of diatomite

Science.gov (United States)

Xiao, Liguang; Pang, Bo

2017-09-01

The volcanic ash activity of diatomite was studied under the conditions of aerobic calcination and vacuum calcination by the combined water rate method, it was characterized by XRD, BET and SEM. The results showed that the volcanic ash activity of diatomite under vacuum conditions was higher than that of aerobic calcination, 600°C vacuum calcination 2h, the combined water rate of diatomite-Ca(OH)2-H2O system was increased from 6.24% to 71.43%, the volcanic ash activity reached the maximum value, the specific surface

RECOVERY OF URANIUM FROM ZIRCONIUM-URANIUM NUCLEAR FUELS

Science.gov (United States)

Gens, T.A.

1962-07-10

An improvement was made in a process of recovering uranium from a uranium-zirconium composition which was hydrochlorinated with gsseous hydrogen chloride at a temperature of from 350 to 800 deg C resulting in volatilization of the zirconium, as zirconium tetrachloride, and the formation of a uranium containing nitric acid insoluble residue. The improvement consists of reacting the nitric acid insoluble hydrochlorination residue with gaseous carbon tetrachloride at a temperature in the range 550 to 600 deg C, and thereafter recovering the resulting uranium chloride vapors. (AEC)

Beryllium and zirconium

International Nuclear Information System (INIS)

Salesse, Marc

1959-01-01

Pure beryllium and zirconium, both isolated at about the same date but more than a century ago remained practically unused for eighty years. Fifteen years ago they were released from this state of inactivity by atomic energy, which made them into current metal a with an annual production which runs into tens of tons for the one and thousands for the other. The reasons for this promotion promise well for the future of the two metals, which moreover will probably find additional uses in other branches of industry. The attraction of beryllium and zirconium for atomic energy is easily explained. The curve of figure 1 gives the price per gram of uranium-235 as a function of enrichment: this price increases by about a factor of 3 on passing from natural uranium (0, 7 percent 235 U) to almost pure uranium-235. Because of their tow capture cross-section beryllium and zirconium make it possible, or at least easier, to use natural uranium and they thus enjoy an advantage the extent of which must be calculated for each reactor or fuel element project, but which is generally considerable. It will be seen later that this advantage should be based on figures which are even more favourable that would appear from the simple ratio 3 of the price of pure uranium- 235 contained in natural uranium. Reprint of a paper published in 'Industries Atomiques' - n. 1-2, 1959

Spray Calciner/In-Can Melter high-level waste solidification technical manual

International Nuclear Information System (INIS)

Larson, D.E.

1980-09-01

This technical manual summarizes process and equipment technology developed at Pacific Northwest Laboratory over the last 20 years for vitrification of high-level liquid waste by the Spray Calciner/In-Can Melter process. Pacific Northwest Laboratory experience includes process development and demonstration in laboratory-, pilot-, and full-scale equipment using nonradioactive synthetic wastes. Also, laboratory- and pilot-scale process demonstrations have been conducted using actual high-level radioactive wastes. In the course of process development, more than 26 tonnes of borosilicate glass have been produced in 75 canisters. Four of these canisters contained radioactive waste glass. The associated process and glass chemistry is discussed. Technology areas described include calciner feed treatment and techniques, calcination, vitrification, off-gas treatment, glass containment (the canister), and waste glass chemistry. Areas of optimization and site-specific development that would be needed to adapt this base technology for specific plant application are indicated. A conceptual Spray Calciner/In-Can Melter system design and analyses are provided in the manual to assist prospective users in evaluating the process for plant application, to provide equipment design information, and to supply information for safety analyses and environmental reports. The base (generic) technology for the Spray Calciner/In-Can Melter process has been developed to a point at which it is ready for plant application

In vitro studies evaluating leaching of mercury from mine waste calcine using simulated human body fluids

Science.gov (United States)

Gray, John E.; Plumlee, Geoffrey S.; Morman, Suzette A.; Higueras, Pablo L.; Crock, James G.; Lowers, Heather A.; Witten, Mark L.

2010-01-01

In vitro bioaccessibility (IVBA) studies were carried out on samples of mercury (Hg) mine-waste calcine (roasted Hg ore) by leaching with simulated human body fluids. The objective was to estimate potential human exposure to Hg due to inhalation of airborne calcine particulates and hand-to-mouth ingestion of Hg-bearing calcines. Mine waste calcines collected from Hg mines at Almadén, Spain, and Terlingua, Texas, contain Hg sulfide, elemental Hg, and soluble Hg compounds, which constitute primary ore or compounds formed during Hg retorting. Elevated leachate Hg concentrations were found during calcine leaching using a simulated gastric fluid (as much as 6200 μg of Hg leached/g sample). Elevated Hg concentrations were also found in calcine leachates using a simulated lung fluid (as much as 9200 μg of Hg leached/g), serum-based fluid (as much as 1600 μg of Hg leached/g), and water of pH 5 (as much as 880 μg of Hg leached/g). The leaching capacity of Hg is controlled by calcine mineralogy; thus, calcines containing soluble Hg compounds contain higher leachate Hg concentrations. Results indicate that ingestion or inhalation of Hg mine-waste calcine may lead to increased Hg concentrations in the human body, especially through the ingestion pathway.

Characterization of magnetic biochar amended with silicon dioxide prepared at high temperature calcination

Directory of Open Access Journals (Sweden)

Baig Shams Ali

2016-09-01

Full Text Available Calcination is considered to increase the hardness of composite material and prevent its breakage for the effective applications in environmental remediation. In this study, magnetic biochar amended with silicon dioxide was calcined at high temperature under nitrogen environment and characterized using various techniques. X-ray diffraction (XRD analysis revealed elimination of Fe3O4 peaks under nitrogen calcination and formation of Fe3Si and iron as major constituents of magnetic biochar-SiO2 composite, which demonstrated its superparamagnetic behavior (>80 A2·kg−1 comparable to magnetic biochar. Thermogravimetric analysis (TGA revealed that both calcined samples generated higher residual mass (>96 % and demonstrated better thermal stability. The presence of various bands in Fourier transform infrared spectroscopy (FT-IR was more obvious and the elimination of H–O–H bonding was observed at high temperature calcination. In addition, scanning electron microscopy (SEM images revealed certain morphological variation among the samples and the presence of more prominent internal and external pores, which then judged the surface area and pore volume of samples. Findings from this study suggests that the selective calcination process could cause useful changes in the material composites and can be effectively employed in environmental remediation measures.

The effect of calcination conditions on the graphitizability of novel synthetic and coal-derived cokes

Science.gov (United States)

Bennett, Barbara Ellen

The effects of calcination heating rate and ultimate calcination temperature upon calcined coke and subsequent graphitic material microstructures were studied for materials prepared from three different precursors. The pitch precursors used were Mitsubishi AR pitch (a synthetic, 100% mesophase pitch), the NMP-extracted portion of a raw coal, and the NMP-extracted fraction of a coal liquefaction residue obtained from an HTI pilot plant. These materials were all green-coked under identical conditions. Optical microscopy confirmed that the Mitsubishi coke was very anisotropic and the HTI coke was nearly as anisotropic. The coke produced from the direct coal extract was very isotropic. Crystalline development during calcination heating was verified by high-temperature x-ray diffraction. Experiments were performed to ascertain the effects of varying calcination heating rate and ultimate temperature. It was determined that calcined coke crystallite size increased with increasing temperature for all three materials but was found to be independent of heating rate. The graphene interplanar spacing decreased with increasing temperature for the isotropic NMP-extract material but increased with increasing temperature for the anisotropic materials---Mitsubishi and HTI cokes. Graphene interplanar spacing was also found to be independent of heating rate. Calcined coke real densities were, likewise, found to be independent of heating rate. The anisotropic cokes (Mitsubishi and HTI) exhibited increasing real density with increasing calcination temperature. The NMP-extract coke increased in density up to 1050°C and then suffered a dramatic reduction in real density when heated to 1250°C. This is indicative of puffing. Since there was no corresponding disruption in the crystalline structure, the puffing phenomena was determined to be intercrystalline rather than intracrystalline. After the calcined cokes were graphitized (under identical conditions), the microstructures were re

Formulation Efforts for Direct Vitrification of INEEL Blend Calcine Waste Simulate: Fiscal Year 2000

Energy Technology Data Exchange (ETDEWEB)

Crum, Jarrod V.; Vienna, John D.; Peeler, David K.; Reamer, I. A.

2001-03-30

This report documents the results of glass formulation efforts for Idaho National Engineering and Environmental Laboratory (INEEL) high level waste (HWL) calcine. Two waste compositions were used during testing. Testing started by using the Run 78 calcine composition and switched to simulated Blend calcine composition when it became available. The goal of the glass formulation efforts was to develop a frit composition that will accept higher waste loading that satisfies the glass processing and product acceptance constraints. 1. Melting temperature of 1125 ? 25?C 2. Viscosity between 2 and 10 Pa?s at the melting temperature 3. Liquidus temperature at least 100?C below the melting temperature 4. Normalized release of B, Li and Na each below 1 g/m2 (per ASTM C 1285-97) Glass formulation efforts tested several frit compositions with variable waste loadings of Run 78 calcine waste simulant. Frit 107 was selected as the primary candidate for processing since it met all process and performance criteria up to 45 mass% waste loading. When the simulated Blend calcine waste composition became available Frits 107 and 108 compositions were retested and again Frit 107 remained the primary candidate. However, both frits suffered a decrease in waste loading when switching from the Run 78 calcine to simulated Blend calcine waste composition. This was due to increase concentrations of both F and Al2O3 along with a decrease in CaO and Na2O in the simulate Blend calcine waste all of which have strong impacts on the glass properties that limit waste loading of this type of waste.

Laser-Based Additive Manufacturing of Zirconium

Directory of Open Access Journals (Sweden)

Himanshu Sahasrabudhe

2018-03-01

Full Text Available Additive manufacturing of zirconium is attempted using commercial Laser Engineered Net Shaping (LENSTM technique. A LENSTM-based approach towards processing coatings and bulk parts of zirconium, a reactive metal, aims to minimize the inconvenience of traditional metallurgical practices of handling and processing zirconium-based parts that are particularly suited to small volumes and one-of-a-kind parts. This is a single-step manufacturing approach for obtaining near net shape fabrication of components. In the current research, Zr metal powder was processed in the form of coating on Ti6Al4V alloy substrate. Scanning electron microscopy (SEM and energy dispersive spectroscopy (EDS as well as phase analysis via X-ray diffraction (XRD were studied on these coatings. In addition to coatings, bulk parts were also fabricated using LENS™ from Zr metal powders, and measured part accuracy.

Quantitative analysis of nickel in zirconium and zircaloy

International Nuclear Information System (INIS)

Rastoix, M.

1957-01-01

A rapid spectrophotometric has been developed for determination of 10 to 1000 ppm of Ni in zirconium and zircaloy using dimethylglyoxime. Iron, copper, tin and chromium, do not interfere at the concentration usually present in zirconium and its alloys. (author) [fr

Techniques for detection of transition phases in calcined alumina

International Nuclear Information System (INIS)

Pandolfelli, V.C.; Folgueras-Dominguez, S.

1987-01-01

Detection of transition phases in alumina, is very important in the receiving control and calcination of aluminium hydroxide. The non alfa or transition phases difficults the processability and causes localized shrinkage on sintering compromising the dimensional and mechanical aspects of the product. In this research using refraction index, absorption of dyes, specific density, X-ray diffraction and scanning electron microscopy, analyses, are done in calcined hydroxides submited to different thermal treatments. The limits and facilities of each technique are discussed and compared. (Author) [pt

Selection of dissolution process for spent fuels and preparation of corrosion test solution simulated to dissolver (contract research)

International Nuclear Information System (INIS)

Motooka, Takafumi; Terakado, Shogo; Koya, Toshio; Hamada, Shozo; Kiuchi, Kiyoshi

2001-03-01

In order to evaluate the reliability of reprocessing equipment materials used in the Rokkasho Reprocessing Plant, we have proceeded a mock-up test and laboratory tests for getting corrosion parameters. In a dissolver made of zirconium, the simulation of test solutions to the practical solution which includes the high concentration of radioactive elements such as FP and TRU is one of the important issues with respect to the life prediction. On this experiment, the dissolution process of spent fuels and the preparation of test solution for evaluating the corrosion resistance of dissolver materials were selected. These processes were tested in the No.3 cell of WASTEF. The test solution for corrosion tests was prepared by adjusting the uranium and nitric acid concentrations. (author)

Continuous precipitation of mineral products: influence of mixing conditions on the co-precipitation of cerium-zirconium mixed oxides

International Nuclear Information System (INIS)

Di Patrizio, Nicolas

2015-01-01

An automated experimental set-up with rapid mixers is used to study the influence of mixing conditions on the co-precipitation of cerium-zirconium mixed oxides. The intensity of mixing is controlled by the inlet flow rates of the reacting solutions. An engulfment model is used to estimate a mixing time from the measurement of a segregation index by the Villermaux-Dushman reaction system. Three geometries of Hartridge Roughton mixers are compared. Mixing performance is better when a separate mixing chamber upstream of a narrower outlet pipe is present. A better mixing decreases the maximal reducibility temperature of the material and increases the crystal strains of the particles calcined at 1100 C. This is probably due to a better homogenization of the particles content. The important incorporation of nitrates in the particle at the outlet of the mixers shows precipitation occurs while the mixing process is not finished. This experimental result was confirmed by numerical simulation and an estimation of sur-saturations during the mixing process. (author)

Immobilization of transition metal ions on zirconium phosphate monolayers

International Nuclear Information System (INIS)

Melezhik, A.V.; Brej, V.V.

1998-01-01

It is shown that ions of transition metals (copper, iron, vanadyl, titanium) are adsorbed on zirconium phosphate monolayers. The zirconium phosphate threshold capacity corresponds to substitution of all protons of hydroxyphosphate groups by equivalent amounts of copper, iron or vanadyl. Adsorption of polynuclear ions is possible in case of titanium. The layered substance with specific surface up to 300 m 2 /g, wherein ultradispersed titanium dioxide particles are intercalirated between zirconium-phosphate layers, is synthesized

Titanium zirconium and hafnium coordination compounds with vanillin thiosemicarbazone

International Nuclear Information System (INIS)

Konunova, Ts.B.; Kudritskaya, S.A.

1987-01-01

Coordination compounds of titanium zirconium and hafnium tetrachlorides with vanillin thiosemicarbazone of MCl 4 x nLig composition, where n=1.5, 4 for titanium and 1, 2, 4 for zirconium and hafnium, are synthesized. Molar conductivity of ethanol solutions is measured; IR spectroscopic and thermochemical investigation are carried out. The supposition about ligand coordination via sulfur and azomethine nitrogen atoms is made. In all cases hafnium forms stable compounds than zirconium

Pyrochemical treatment of Idaho Chemical Processing Plant high-level waste calcine

International Nuclear Information System (INIS)

Todd, T.A.; DelDebbio, J.A.; Nelson, L.O.; Sharpsten, M.R.

1993-01-01

The Idaho Chemical Processing Plant (ICPP), located at the Idaho National Engineering Laboratory (INEL), has reprocessed irradiated nuclear fuels for the US Department of Energy (DOE) since 1951 to recover uranium, krypton-85, and isolated fission products for interim treatment and immobilization. The acidic radioactive high-level liquid waste (HLLW) is routinely stored in stainless steel tanks and then, since 1963, calcined to form a dry granular solid. The resulting high-level waste (HLW) calcine is stored in seismically hardened stainless steel bins that are housed in underground concrete vaults. A research and development program has been established to determine the feasibility of treating ICPP HLW calcine using pyrochemical technology.This technology is described

The chemical vapor deposition of zirconium carbide onto ceramic substrates

International Nuclear Information System (INIS)

Glass A, John Jr.; Palmisiano, Nick Jr.; Welsh R, Edward

1999-01-01

Zirconium carbide is an attractive ceramic material due to its unique properties such as high melting point, good thermal conductivity, and chemical resistance. The controlled preparation of zirconium carbide films of superstoichiometric, stoichiometric, and substoichiometric compositions has been achieved utilizing zirconium tetrachloride and methane precursor gases in an atmospheric pressure high temperature chemical vapor deposition system

Modelling of Zirconium and Hafnium separation using continuous annular chromatography

International Nuclear Information System (INIS)

Moch-Setyadji; Endang Susiantini

2014-01-01

Nuclear degrees of zirconium in the form of a metal alloy is the main material for fuel cladding of NPP. Zirconium is also used as sheathing UO 2 kernel in the form of ZrC as a substitute of SiC in the fuel elements of High Temperature Reactor (HTR). Difficulty separating hafnium from zirconium because it has a lot of similarities in the chemical properties of Zr and Hf. Annular chromatography is a device that can be used for separating of zirconium and hafnium to obtain zirconium nuclear grade. Therefore, it is necessary to construct the mathematical modelling that can describe the separation of zirconium and hafnium in the annular chromatography containing anion resin dowex-1X8. The aim of research is to perform separation simulation by using the equilibrium model and mass transfer coefficient resulted from research. Zr and Hf feed used in this research were 26 and 1 g/l, respectively. Height of resin (L), angular velocity (ω) and the superficial flow rate (uz) was varied to determine the effect of each parameter on the separation of Zr and Hf. By using Kd and Dv values resulted previous research. Simulation results showed that zirconium and hafnium can be separated using a continuous annular chromatography with high resin (long bed) 50 cm, superficial flow rate of 0.001 cm/s, the rotation speed of 0.006 rad/min and 20 cm diameter annular. In these conditions the results obtained zirconium concentration of 10,303.226 g/m 3 and hafnium concentration of 12.324 g/m 3 (ppm). (author)

46 CFR 148.04-17 - Petroleum coke, calcined, at 130 °F or above.

Science.gov (United States)

2010-10-01

... 46 Shipping 5 2010-10-01 2010-10-01 false Petroleum coke, calcined, at 130 °F or above. 148.04-17...-17 Petroleum coke, calcined, at 130 °F or above. (a) The requirements of this part do not apply to bulk shipments of petroleum coke, calcined, on any vessel when the material is less than 130 °F. (b...

Young's modulus of crystal bar zirconium and zirconium alloys (zircaloy-2, zircaloy-4, zirconium-2.5wt% niobium) to 1000 K

International Nuclear Information System (INIS)

Rosinger, H.E.; Ritchie, I.G.; Shillinglaw, A.J.

1975-09-01

This report contains experimentally determined data on the dynamic elastic moduli of zircaloy-2, zircaloy-4, zirconium-2.5wt% niobium and Marz grade crystal bar zirconium. Data on both the dynamic Young's moduli and shear moduli of the alloys have been measured at room temperature and Young's modulus as a function of temperature has been determined over the temperature range 300 K to 1000 K. In every case, Young's modulus decreases linearly with increasing temperature and is expressed by an empirical equation fitted to the data. Differences in Young's modulus values determined from specimens with longitudinal axes parallel and perpendicular to the rolling direction are small, as are the differences between Young's moduli determined from strip, bar stock and fuel sheathing. (author)

In vitro assessment of artifacts induced by titanium, titanium-zirconium and zirconium dioxide implants in cone-beam computed tomography.

Science.gov (United States)

Sancho-Puchades, Manuel; Hämmerle, Christoph H F; Benic, Goran I

2015-10-01

The aim of this study was to test whether or not the intensity of artifacts around implants in cone-beam computed tomography (CBCT) differs between titanium, titanium-zirconium and zirconium dioxide implants. Twenty models of a human mandible, each containing one implant in the single-tooth gap position 45, were cast in dental stone. Five test models were produced for each of the following implant types: titanium 4.1 mm diameter (Ti4.1 ), titanium 3.3 mm diameter (Ti3.3 ), titanium-zirconium 3.3 mm diameter (TiZr3.3 ) and zirconium dioxide 3.5-4.5 mm diameter (ZrO3.5-4.5 ) implants. For control purposes, three models without implants were produced. Each model was scanned using a CBCT device. Gray values (GV) were recorded at eight circumferential positions around the implants at 0.5 mm, 1 mm and 2 mm from the implant surface (GVT est ). GV were assessed in the corresponding volumes of interest (VOI) in the control models without implants (GVC ontrol ). Differences of gray values (ΔGV) between GVT est and GVC ontrol were calculated as percentages. One-way ANOVA and post hoc tests were applied to detect differences between implant types. Mean ΔGV for ZrO3.5-4.5 presented the highest absolute values, generally followed by TiZr3.3 , Ti4.1 and Ti3.3 implants. The differences of ΔGV between ZrO3.5-4.5 and the remaining groups were statistically significant in the majority of the VOI (P ≤ 0.0167). ΔGV for TiZr3.3 , Ti4.1 and Ti3.3 implants did not differ significantly in the most VOI. For all implant types, ΔGV showed positive values buccally, mesio-buccally, lingually and disto-lingually, whereas negative values were detected mesially and distally. Zirconium dioxide implants generate significantly more artifacts as compared to titanium and titanium-zirconium implants. The intensity of artifacts around zirconium dioxide implants exhibited in average the threefold in comparison with titanium implants. © 2014 John Wiley & Sons A/S. Published by John Wiley

Spectrophotometric titration of sulfates in the presence of zirconium

International Nuclear Information System (INIS)

Kuznetsov, V.V.; Kotova, S.S.; Molokanova, L.G.; Chekmarev, A.M.; Yagodin, G.A.

1978-01-01

The procedure has been proposed for express determination of sulphate ions in the presence of zirconium by spectrophotometric titration with the use of barium chloride and nitrochromazo as an indicator. The procedure is based on bonding zirconium into a more stable complex with EDTA (ethylenediaminotetraacetic acid). The presence of excess of EDTA and zirconium (4) complexonate in the solution being titrated does not affect the titration curve shape and the character of break on the curve in the equivalence point. A complete demasking of SO 4 2- is observed in the case of 1O-fold excess of EDTA with respect to zirconium (4). Statistic evaluation of the method has shown that the results of titration can be distorted by chance errors only

Calcination effects on CeZrOx geometry and styrene production from ethylbenzene

NARCIS (Netherlands)

Kovacevic, M.; Brunet Espinosa, Roger; Lefferts, Leonardus; Mojet, Barbara

2014-01-01

A series of CeZrOx catalysts was prepared by calcination of hydrothermally obtained metal oxide precipitate at increasing temperatures. The samples were characterized by HRSEM, XRD and Raman spectroscopy, showing a change in morphology and particle size as a function of calcination temperature.

Final safety-analysis report for the Fifth Calcined Solids Storage Facility

International Nuclear Information System (INIS)

1982-01-01

Radioactive aqueous wastes generated by the solvent extraction of uranium from expended fuels at ICPP will be calcined in the New Waste Calcining Facility (NWCF). The calcined solids are pneumatically transferred to stainless steel bins enclosed in concrete vaults for interim storage of up to 500 years. The Fifth Calcined Solids Storage Facility (CSSF) provides 1000 m 3 of storage and consists of seven annular stainless steel bins inside a reinforced concrete vault set on bedrock. Storage of calcined solids is essentially a passive operation with very little opportunity for release of radionuclides and with no potential for criticality. There will be no potential for fire or explosion. Shielding has been designed to assure that the radiation levels at the vault exterior surfaces will be limited to less than 0.5 mRem/h. A sump in the vault floor will collect any in-leakage that may occur. Any water that collects in the sump will be sampled then removed with the sump jet. There will be an extremely small chance of release of radioactive particulates into the atmosphere as a result of a bin leak. The Design Basis Accident (DBA) postulates the spill of solids from an eroded fill line into the vault coupled with a failure of the vault cooling air radiation monitor. For the DBA, the maximum calculated radiation dose to an exposed individual near the site boundary is less than 1.2 μRem to the bone and lung

Preparation of plutonium waste forms with ICPP calcined high-level waste

Energy Technology Data Exchange (ETDEWEB)

Staples, B.A.; Knecht, D.A. [Lockheed Idaho Technologies Co., Idaho Falls, ID (United States); O`Holleran, T.P. [Argonne National Lab.-West, Idaho Falls, ID (United States)] [and others

1997-05-01

Glass and glass-ceramic forms developed for the immobilization of calcined high-level wastes generated by Idaho Chemical Processing Plant (ICPP) fuel reprocessing activities have been investigated for ability to immobilize plutonium and to simultaneously incorporate calcined waste as an anti-proliferation barrier. Within the forms investigated, crystallization of host phases result in an increased loading of plutonium as well as its incorporation into potentially more durable phases than the glass. The host phases were initially formed and characterized with cerium (Ce{sup +4}) as a surrogate for plutonium (Pu{sup +4}) and samarium as a neutron absorber for criticality control. Verification of the surrogate testing results were then performed replacing cerium with plutonium. All testing was performed with surrogate calcined high-level waste. The results of these tests indicated that a potentially useful host phase, based on zirconia, can be formed either by devitrification or solid state reaction in the glass studied. This phase incorporates plutonium as well as samarium and the calcined waste becomes part of the matrix. Its ease of formation makes it potentially useful in excess plutonium dispositioning. Other durable host phases for plutonium and samarium, including zirconolite and zircon have been formed from zirconia or alumina calcine through cold press-sintering techniques and hot isostatic pressing. Host phase formation experiments conducted through vitrification or by cold press-sintering techniques are described and the results discussed. Recommendations are given for future work that extends the results of this study.

Preparation of plutonium waste forms with ICPP calcined high-level waste

International Nuclear Information System (INIS)

Staples, B.A.; Knecht, D.A.; O'Holleran, T.P.

1997-05-01

Glass and glass-ceramic forms developed for the immobilization of calcined high-level wastes generated by Idaho Chemical Processing Plant (ICPP) fuel reprocessing activities have been investigated for ability to immobilize plutonium and to simultaneously incorporate calcined waste as an anti-proliferation barrier. Within the forms investigated, crystallization of host phases result in an increased loading of plutonium as well as its incorporation into potentially more durable phases than the glass. The host phases were initially formed and characterized with cerium (Ce +4 ) as a surrogate for plutonium (Pu +4 ) and samarium as a neutron absorber for criticality control. Verification of the surrogate testing results were then performed replacing cerium with plutonium. All testing was performed with surrogate calcined high-level waste. The results of these tests indicated that a potentially useful host phase, based on zirconia, can be formed either by devitrification or solid state reaction in the glass studied. This phase incorporates plutonium as well as samarium and the calcined waste becomes part of the matrix. Its ease of formation makes it potentially useful in excess plutonium dispositioning. Other durable host phases for plutonium and samarium, including zirconolite and zircon have been formed from zirconia or alumina calcine through cold press-sintering techniques and hot isostatic pressing. Host phase formation experiments conducted through vitrification or by cold press-sintering techniques are described and the results discussed. Recommendations are given for future work that extends the results of this study

Study of the uranium-zirconium diffusion; Etude de la diffusion uranium-zirconium

Energy Technology Data Exchange (ETDEWEB)

Adda, Y; Mairy, C; Bouchet, P [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

1957-07-01

The intermetallic diffusion of uranium fuel and zirconium used as cladding is studied. Intermetallic diffusion can occur during the cladding of uranium rods and uranium can penetrate the zirconium cladding. Different parameters are involved in this mechanism as structure and mechanical properties of the diffusion area as well as presence of impurities in the metal. The uses of different analysis techniques (micrography, Castaing electronic microprobe, microhardness and autoradiography) have permitted to determine with great accuracy the diffusion coefficient in gamma phase (body centered cubic system) and the results have given important information on the intermetallic diffusion mechanisms. The existence of the Kirkendall effect in the U-Zr diffusion is also an argument in favor of the generality of the diffusion mechanism by vacancies in body centered cubic system. (M.P.)

CFD Modelling and Experimental Testing of Thermal Calcination of Kaolinite Rich Clay Particles - An Effort towards Green Concrete

DEFF Research Database (Denmark)

Gebremariam, Abraham Teklay

Cement industry is one of the major industrial emitters of greenhouse gases, generating 5-7% of the total anthropogenic CO2 emissions. Consequently, use of supplementary cementitious materials (SCM) to replace part of the CO2-intensive cement clinker is an attractive way to mitigate CO2 emissions...... from cement industry. SCMs based on industrial byproducts like fly ashes and slags are subject to availability problems. Yet clays are the most ubiquitous material on earth's crust. Thus, properly calcined clays are a very promising candidate for SCMs to produce green cements. Calcination...... property of the calcined clay material, among which is the density of calcines. By using the variation in density of calcines, an optimum residence time has been marked. At this time the calcines display a minimum density that corresponds to the most dehydroxylated calcines. The behavior of flash calcined...

Effect of calcination temperature on microstructure and electrochemical performance of lithium-rich layered oxide cathode materials

International Nuclear Information System (INIS)

Ma, Quanxin; Peng, Fangwei; Li, Ruhong; Yin, Shibo; Dai, Changsong

2016-01-01

Highlights: • A series of Li-rich layered oxide cathode materials (Li_1_._2Mn_0_._5_6Ni_0_._1_6Co_0_._0_8O_2) were successfully synthesized via a two-step synthesis method. • The effects of calcination temperature on the cathode materials were researched in detail. • A well-crystallized layered structure was obtained as the calcination temperature increased. • The samples calcined in a range of 850–900 °C exhibited excellent electrochemical performance. - Abstract: Lithium-rich layered oxide cathode materials (Li_1_._2Mn_0_._5_6Ni_0_._1_6Co_0_._0_8O_2 (LLMO)) were synthesized via a two-step synthesis method involving co-precipitation and high-temperature calcination. The effects of calcination temperature on the cathode materials were studied in detail. Structural and morphological characterizations revealed that a well-crystallized layered structure was obtained at a higher calcination temperature. Electrochemical performance evaluation revealed that a cathode material obtained at a calcination temperature of 850 °C delivered a high initial discharge capacity of 266.8 mAh g"−"1 at a 0.1 C rate and a capacity retention rate of 95.8% after 100 cycles as well as excellent rate capability. Another sample calcinated at 900 °C exhibited good cycling stability. It is concluded that the structural stability and electrochemical performance of Li-rich layered oxide cathode materials were strongly dependent on calcination temperatures. The results suggest that a calcination temperature in a range of 850–900 °C could promote electrochemical performance of this type of cathode materials.

Effect of calcination temperature on microstructure and electrochemical performance of lithium-rich layered oxide cathode materials

Energy Technology Data Exchange (ETDEWEB)

Ma, Quanxin; Peng, Fangwei; Li, Ruhong; Yin, Shibo; Dai, Changsong, E-mail: changsd@hit.edu.cn

2016-11-15

Highlights: • A series of Li-rich layered oxide cathode materials (Li{sub 1.2}Mn{sub 0.56}Ni{sub 0.16}Co{sub 0.08}O{sub 2}) were successfully synthesized via a two-step synthesis method. • The effects of calcination temperature on the cathode materials were researched in detail. • A well-crystallized layered structure was obtained as the calcination temperature increased. • The samples calcined in a range of 850–900 °C exhibited excellent electrochemical performance. - Abstract: Lithium-rich layered oxide cathode materials (Li{sub 1.2}Mn{sub 0.56}Ni{sub 0.16}Co{sub 0.08}O{sub 2} (LLMO)) were synthesized via a two-step synthesis method involving co-precipitation and high-temperature calcination. The effects of calcination temperature on the cathode materials were studied in detail. Structural and morphological characterizations revealed that a well-crystallized layered structure was obtained at a higher calcination temperature. Electrochemical performance evaluation revealed that a cathode material obtained at a calcination temperature of 850 °C delivered a high initial discharge capacity of 266.8 mAh g{sup −1} at a 0.1 C rate and a capacity retention rate of 95.8% after 100 cycles as well as excellent rate capability. Another sample calcinated at 900 °C exhibited good cycling stability. It is concluded that the structural stability and electrochemical performance of Li-rich layered oxide cathode materials were strongly dependent on calcination temperatures. The results suggest that a calcination temperature in a range of 850–900 °C could promote electrochemical performance of this type of cathode materials.

Uranium (Vi) sorption onto zirconium diphosphate chemically modified

International Nuclear Information System (INIS)

Garcia G, N.; Ordonez R, E.

2010-10-01

This work deals with the uranium (Vi) speciation after sorption onto zirconium diphosphate (ZrP 2 O 7 ) surface, hydrated and in a surface modified with organic acids. Oxalic and citric acids were chosen to modify the ZrP 2 O 7 surface because they have poly carboxylic groups and they mimic the organic matter in nature. Thus the interest of this work is to evaluate the uranium (Vi) sorption edge at different s ph values in natural and modified surfaces. The luminescence technique (fluorescence and phosphorescence, respectively) was used for the quantification and speciation of uranyl sorbed at the zirconium diphosphate interface. The fluorescence experiment, showed that adsorption of uranyl on surface of zirconium diphosphate tends to 100%. The speciation shows that there are different complexes in surface which were formed between zirconium diphosphate and uranyl, since it is produced a displacement of wavelength in fluorescence spectra of each system. (Author)

Pyrochemical separation of radioactive components from inert materials in ICPP high-level calcined waste

International Nuclear Information System (INIS)

Del Debbio, J.A.; Nelson, L.O.; Todd, T.A.

1995-05-01

Since 1963, calcination of aqueous wastes from reprocessing of DOE-owned spent nuclear fuels has resulted in the accumulation of approximately 3800 m 3 of high-level waste (HLW) at the Idaho Chemical Processing Plant (ICPP). The waste is in the form of a granular solid called calcine and is stored on site in stainless steel bins which are encased in concrete. Due to the leachability of 137 Cs and 90 Sr and possibly other radioactive components, the calcine is not suitable for final disposal. Hence, a process to immobilize calcine in glass is being developed. Since radioactive components represent less than 1 wt % of the calcine, separation of actinides and fission products from inert components is being considered to reduce the volume of HLW requiring final disposal. Current estimates indicate that compared to direct vitrification, a volume reduction factor of 10 could result in significant cost savings. Aqueous processes, which involve calcine dissolution in nitric acid followed by separation of actinide and fission products by solvent extraction and ion exchange methods, are being developed. Pyrochemical separation methods, which generate small volumes of aqueous wastes and do not require calcine dissolution, have been evaluated as alternatives to aqueous processes. This report describes three proposed pyrochemical flowsheets and presents the results of experimental studies conducted to evaluate their feasibility. The information presented is a consolidation of three reports, which should be consulted for experimental details

Minimalistic Liquid-Assisted Route to Highly Crystalline α-Zirconium Phosphate.

Science.gov (United States)

Cheng, Yu; Wang, Xiaodong Tony; Jaenicke, Stephan; Chuah, Gaik-Khuan

2017-08-24

Zirconium phosphates have potential applications in areas of ion exchange, catalysis, photochemistry, and biotechnology. However, synthesis methodologies to form crystalline α-zirconium phosphate (Zr(HPO 4 ) 2 ⋅H 2 O) typically involve the use of excess phosphoric acid, addition of HF or oxalic acid and long reflux times or hydrothermal conditions. A minimalistic sustainable route to its synthesis has been developed by using only zirconium oxychloride and concentrated phosphoric acid to form highly crystalline α-zirconium phosphate within hours. The morphology can be changed from platelets to rod-shaped particles by fluoride addition. By varying the temperature and time, α-zirconium phosphate with particle sizes from nanometers to microns can be obtained. Key features of this minimal solvent synthesis are the excellent yields obtained with high atom economy under mild conditions and ease of scalability. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fluidized-bed calcination of LWR fuel-reprocessing HLLW: requirements and potential for off-gas cleanup

International Nuclear Information System (INIS)

Schindler, R.E.

1979-01-01

Fluidized-bed solidification (calcination) was developed on a pilot scale for a variety of simulated LWR high-level liquid-waste (HLLW) and blended high-level and intermediate-level liquid-waste (ILLW) compositions. It has also been demonstrated with ICPP fuel-reprocessing waste since 1963 in the Waste Calcining Facility (WCF) at gross feed rates of 5 to 12 m 3 /day. A fluidized-bed calciner produces a relatively large volume of off-gas. A calciner solidifying 6 m 3 /day of liquid waste would generate about 13 standard m 3 /min of off-gas containing 10 to 20 g of entrained solids per standard m 3 of off-gas. Use of an off-gas system similar to that of the WCF could provide an overall process decontamination factor for particulates of about 2 x 10 10 . A potential advantage of fluidized-bed calcination over other solidification methods is the ability to control ruthenium volatilization from the calciner at less than 0.01% by calcining at 500 0 C or above. Use of an off-gas system similar to that of the WCF would provide an overall process decontamination factor for volatile ruthenium of greater than 1.6 x 10 7

Electrochemical impedance spectroscopic study of passive zirconium

Energy Technology Data Exchange (ETDEWEB)

Ai Jiahe; Chen Yingzi [Center for Electrochemical Science and Technology, Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States); Urquidi-Macdonald, Mirna [Department of Engineering Science and Mechanics, Pennsylvania State University, University Park, PA 16802 (United States); Macdonald, Digby D. [Center for Electrochemical Science and Technology, Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States)], E-mail: ddm2@psu.edu

2008-09-30

Spent, unreproccessed nuclear fuel is generally contained within the operational fuel sheathing fabricated from a zirconium alloy (Zircaloy 2, Zircaloy 4, or Zirlo) and is then stored in a swimming pool and/or dry storage facilities until permanent disposal in a licensed repository. During this period, which begins with irradiation of the fuel in the reactor during operation, the fuel sheathing is exposed to various, aggressive environments. The objective of the present study was to characterize the nature of the passive film that forms on pure zirconium in contact with an aqueous phase [0.1 M B(OH){sub 3} + 0.001 M LiOH, pH 6.94] at elevated temperatures (in this case, 250 deg. C), prior to storage, using electrochemical impedance spectroscopy (EIS) with the data being interpreted in terms of the point defect model (PDM). The results show that the corrosion resistance of zirconium in high temperature, de-aerated aqueous solutions is dominated by the outer layer. The extracted model parameter values can be used in deterministic models for predicting the accumulation of general corrosion damage to zirconium under a wide range of conditions that might exist in some repositories.

Quantitative analysis of calcined fertilizers by X-ray diffraction patterns

International Nuclear Information System (INIS)

Cekinski, E.

1987-01-01

An X-ray diffraction pattern method for quantitative analyses of phosphate fertilizers obtained by calcination of a misture of Anitapolis phosphate concentrate and sodium carbonate is described. The method consists in plotting a calibration curve, using spinel (MgAl 2 O 4 ) as internal standard, of the phases that were formed by calcination, sintetized in laboratory. The tests conducted in order to avail the method accuracy showed good correlation between the obtained data and the real values. (author) [pt

Some recent trends in the use of zirconium alloys for nuclear service

International Nuclear Information System (INIS)

Balaramamoorthy, K.

1992-01-01

Without any exception nuclear power reactors particularly the water cooled ones, operating in the World use natural or slightly enriched uranium oxide fuel pellets with zirconium alloy cladding. While the zirconium alloys have proven to be successful in their designed usage, a desire for longer lifetimes of core components and increased duty cycle puts more demand on materials performance. This demand has led to more in depth studies of phenomena associated with zirconium alloy corrosion mechanism, fine tuning of the zirconium alloy composition, development of fabrication techniques and to the evaluation of newer zirconium alloys for critical applications. (author). 5 refs., 32 figs

Total oxidation of toluene over calcined trimetallic hydrotalcites type catalysts

Energy Technology Data Exchange (ETDEWEB)

Palacio, Luz A. [Instituto Superior Tecnico, IBB - Centro de Engenharia Biologica e Quimica, Universidade Tecnica de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Grupo Catalizadores y Adsorbentes, Universidad de Antioquia 1-317, A.A. 1226 Medellin (Colombia); Velasquez, Juliana; Echavarria, Adriana [Grupo Catalizadores y Adsorbentes, Universidad de Antioquia 1-317, A.A. 1226 Medellin (Colombia); Faro, Arnaldo [Departamento de Fisicoquimica, Instituto de Quimica, Universidade Federal do Rio de Janeiro, Ilha do Fundao, CT bloco A, Rio de Janeiro (Brazil); Ramoa Ribeiro, F. [Instituto Superior Tecnico, IBB - Centro de Engenharia Biologica e Quimica, Universidade Tecnica de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Ribeiro, M. Filipa, E-mail: filipa.ribeiro@ist.utl.pt [Instituto Superior Tecnico, IBB - Centro de Engenharia Biologica e Quimica, Universidade Tecnica de Lisboa, Av. Rovisco Pais, 1049-001 Lisboa (Portugal)

2010-05-15

Two trimetallic ZnCuAl and MnCuAl hydrotalcites have been successfully synthesized by a co-precipitation method. The manganese based material was identified as a new hydrotalcite phase. Both lamellar precursors were calcined at 450 and 600 deg. C and the resulting catalysts were tested on reaction of total oxidation of toluene. The solids were characterized by X-ray diffraction, thermal analysis, atomic absorption spectroscopy, Fourier transformed infrared spectroscopy, N{sub 2} adsorption and H{sub 2} temperature-programmed reduction. It was found that ZnCuAl materials are composed of copper and zinc oxides supported on alumina; while MnCuAl ones comprise basically spinel phases, which were not completely identified. The catalytic behavior of the calcined samples showed that Mn hydrotalcite calcined at 450 deg. C exhibited the best catalytic performance that corresponds to 100% toluene conversion into CO{sub 2} at about 300 deg. C.

Total oxidation of toluene over calcined trimetallic hydrotalcites type catalysts

International Nuclear Information System (INIS)

Palacio, Luz A.; Velasquez, Juliana; Echavarria, Adriana; Faro, Arnaldo; Ramoa Ribeiro, F.; Ribeiro, M. Filipa

2010-01-01

Two trimetallic ZnCuAl and MnCuAl hydrotalcites have been successfully synthesized by a co-precipitation method. The manganese based material was identified as a new hydrotalcite phase. Both lamellar precursors were calcined at 450 and 600 deg. C and the resulting catalysts were tested on reaction of total oxidation of toluene. The solids were characterized by X-ray diffraction, thermal analysis, atomic absorption spectroscopy, Fourier transformed infrared spectroscopy, N 2 adsorption and H 2 temperature-programmed reduction. It was found that ZnCuAl materials are composed of copper and zinc oxides supported on alumina; while MnCuAl ones comprise basically spinel phases, which were not completely identified. The catalytic behavior of the calcined samples showed that Mn hydrotalcite calcined at 450 deg. C exhibited the best catalytic performance that corresponds to 100% toluene conversion into CO 2 at about 300 deg. C.

Translucency and Strength of High Translucency Monolithic Zirconium Oxide Materials

Science.gov (United States)

2016-05-17

Zirconium -Oxide Materials presented at/published to the Journal of General Dentistry with MDWI 41-108, and has been assigned local file #16208. 2...Zirconia-Oxide Materials 6. TITLE OF MATERIAL TO BE PUBLISHED OR PRESENTED: Translucency and Strength of High-Translucency Monolithic Zirconium -Oxide...OBSOLETE 48. DATE Page 3 of 3 Pages Translucency and Strength of High-Translucency Monolithic Zirconium -Oxide Materials Abstract Dental materials

Synthesis of type A zeolite from calcinated kaolin

International Nuclear Information System (INIS)

Rodrigues, E.C.; Neves, R.F.; Souza, J.A.S.; Moraes, C.G.; Macedo, E.N.

2011-01-01

The mineral production has caused great concern in environmental and industrial scenario due to the effects caused to the environment. The industries of processing kaolin for paper are important economically for the state of Para, but produce huge quantities of tailings, which depend on large areas to be stocked. This material is rich in silico-aluminates can be recycled and used as raw material for other industries. The objective is to synthesize zeolite A at different temperatures of calcination and synthesis. The starting materials and synthesis of zeolite A have been identified and characterized through analysis of X-ray diffraction (DRX) and scanning electron microscopy (MEV). The synthesis process of zeolite A, using as source of silica and the aluminum metakaolin, which was calcined at temperatures of 700 ° C and 800 ° C for 2 hours of landing in a burning furnace type muffle. Observed in relation to the calcination of kaolin as the main phase, the metakaolin. This is just a removal of water from its structure, so we opted for the lower temperature, less energy consumption. The synthesis process of zeolite A, produced good results for the formation of zeolites type A, which were characterized with high purities. (author)

Biodiesel production from waste cooking oil using calcined scallop shell as catalyst

International Nuclear Information System (INIS)

Sirisomboonchai, Suchada; Abuduwayiti, Maidinamu; Guan, Guoqing; Samart, Chanatip; Abliz, Shawket; Hao, Xiaogang; Kusakabe, Katsuki; Abudula, Abuliti

2015-01-01

Highlights: • Calcined scallop shell was used as low-cost and effective catalyst for biodiesel production. • BDF yield from waste cooking oil reached 86% at 65 °C with a catalyst loading amount of 5 wt%. • Calcined scallop shell showed good reusability. • Calcium glyceroxide played an important role on the reusability of calcined scallop shell. • Water in the waste cooking oil had negative effect on the catalytic activity of calcined scallop shell. - Abstract: Transesterification of waste cooking oil (WCO) and methanol by using calcined scallop shell (CSS) as catalyst was carried out in a closed system for biodiesel fuel (BDF) production. It is found that the optimum calcination temperature for the preparation of CSS was 1000 °C. The effects of transesterification temperature, reaction time, methanol/oil molar ratio and catalyst loading amount on the BDF yield were investigated. Compared with the commercial CaO, CSS showed higher catalytic activity and the BDF yield reached 86% at 65 °C with a catalyst loading amount of 5 wt% (WCO basis) and a reaction time of 2 h. The catalyst was reused for 5 cycles whilst the BDF yield decreased 23%. It is found that CaO in CSS was transferred to calcium glyceroxide after the transesterification reaction, and calcium glyceroxide also showed good catalytic activity and reusability. Furthermore, Water content in WCO had negative effect on BDF yield. It is found that BDF yield reduced 15% due to the occurring of saponification when the water content was increased from 0.64% to 2.48%. It is expected that CCS can be used as an alternative and cheap catalyst for the biodiesel production

International strategic minerals inventory summary report; zirconium

Science.gov (United States)

Towner, R.R.

1992-01-01

Zircon, a zirconium silicate, is currently the most important commercial zirconium-bearing mineral. Baddeleyite, a natural form of zirconia, is less important but has some specific end uses. Both zircon and baddeleyite occur in hard-rock and placer deposits, but at present all zircon production is from placer deposits. Most baddeleyite production is from hard-rock deposits, principally as a byproduct of copper and phosphate-rock mining. World zirconium resources in identified, economically exploitable deposits are about 46 times current production rates. Of these resources, some 71 percent are in South Africa, Australia, and the United States. The principal end uses of zirconium minerals are in ceramic applications and as refractories, abrasives, and mold linings in foundries. A minor amount, mainly of zircon, is used for the production of hafnium-free zirconium metal, which is used principally for sheathing fuel elements in nuclear reactors and in the chemical-processing industry, aerospace engineering, and electronics. Australia and South Africa are the largest zircon producers and account for more than 70 percent of world output; the United States and the Soviet Union account for another 20 percent. South Africa accounts for almost all the world's production of baddeleyite, which is about 2 percent of world production of contained zirconia. Australia and South Africa are the largest exporters of zircon. Unless major new deposits are developed in countries that have not traditionally produced zircon, the pattern of world production is unlikely to change by 2020. The proportions, however, of production that come from existing producing countries may change somewhat.

Process for optimizing titanium and zirconium additions to aluminum welding consumables

International Nuclear Information System (INIS)

Dvornak, M.J.; Frost, R.H.

1992-01-01

This patent describes a process for manufacturing an aluminum welding consumable. It comprises: creating an aluminum melt; adding to the aluminum melt solid pieces of a master alloy, comprising aluminum and a weld-enhancing additive to form a mixture, wherein the weld-enhancing additive being a material selected from the group consisting of titanium and zirconium, so that the weld-enhancing additive exists in the alloy prior to addition to the melt in the form of intermetallic particles relatively large in size and small in number, and after addition to the melt the weld-enhancing additive exists in the form of fractured intermetallic particles of refined size having dissolved fractured interfaces, casting the mixture into a chill mold to form an ingot; reducing the ingot to rods of rough wire dimension by cold rolling; annealing the reduced rods; and drawing the rods into wire

CO{sub 2} capture behavior of shell during calcination/carbonation cycles

Energy Technology Data Exchange (ETDEWEB)

Li, Y.J.; Zhao, C.S.; Chen, H.C.; Duan, L.B.; Chen, X.P. [School of Energy and Environment, Southeast University, Nanjing (China)

2009-08-15

The cyclic carbonation performances of shells as CO{sub 2} sorbents were investigated during multiple calcination/carbonation cycles. The carbonation kinetics of the shell and limestone are similar since they both exhibit a fast kinetically controlled reaction regime and a diffusion controlled reaction regime, but their carbonation rates differ between these two regions. Shell achieves the maximum carbonation conversion for carbonation at 680-700 C. The mactra veneriformis shell and mussel shell exhibit higher carbonation conversions than limestone after several cycles at the same reaction conditions. The carbonation conversion of scallop shell is slightly higher than that of limestone after a series of cycles. The calcined shell appears more porous than calcined limestone, and possesses more pores >230 nm, which allow large CO{sub 2} diffusion-carbonation reaction rates and higher conversion due to the increased surface area of the shell. The pores of the shell that are greater than 230 nm do not sinter significantly. The shell has more sodium ions than limestone, which probably leads to an improvement in the cyclic carbonation performance during the multiple calcination/carbonation cycles. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

The nitric acid decomposition of calcined danburite concentrate of Ak-Arkhar Deposit

International Nuclear Information System (INIS)

Kurbonov, A.S.; Mamatov, E.D.; Suleymani, M.; Borudzherdi, A.; Mirsaidov, U.M.

2011-01-01

Present article is devoted to nitric acid decomposition of calcined danburite concentrate of Ak-Arkhar Deposit of Tajikistan. The obtaining of boric acid from pre backed danburite concentrate by decomposition of nitric acid was studied. The chemical composition of danburite concentrate was determined. The laboratory study of danburite leaching by nitric acid was conducted. The influence of temperature, process duration, nitric acid concentration on nitric acid decomposition of calcined danburite concentrate of Ak-Arkhar Deposit was studied as well. The optimal conditions of nitric acid decomposition of calcined danburite concentrate of Ak-Arkhar Deposit, including temperature, process duration, nitric acid concentration and particle size were proposed.

Screening Level Risk Assessment for the New Waste Calcining Facility

Energy Technology Data Exchange (ETDEWEB)

M. L. Abbott; K. N. Keck; R. E. Schindler; R. L. VanHorn; N. L. Hampton; M. B. Heiser

1999-05-01

This screening level risk assessment evaluates potential adverse human health and ecological impacts resulting from continued operations of the calciner at the New Waste Calcining Facility (NWCF) at the Idaho Nuclear Technology and Engineering Center (INTEC), Idaho National Engineering and Environmental Laboratory (INEEL). The assessment was conducted in accordance with the Environmental Protection Agency (EPA) report, Guidance for Performing Screening Level Risk Analyses at Combustion Facilities Burning Hazardous Waste. This screening guidance is intended to give a conservative estimate of the potential risks to determine whether a more refined assessment is warranted. The NWCF uses a fluidized-bed combustor to solidify (calcine) liquid radioactive mixed waste from the INTEC Tank Farm facility. Calciner off volatilized metal species, trace organic compounds, and low-levels of radionuclides. Conservative stack emission rates were calculated based on maximum waste solution feed samples, conservative assumptions for off gas partitioning of metals and organics, stack gas sampling for mercury, and conservative measurements of contaminant removal (decontamination factors) in the off gas treatment system. Stack emissions were modeled using the ISC3 air dispersion model to predict maximum particulate and vapor air concentrations and ground deposition rates. Results demonstrate that NWCF emissions calculated from best-available process knowledge would result in maximum onsite and offsite health and ecological impacts that are less then EPA-established criteria for operation of a combustion facility.

In Vitro Studies Evaluating Leaching of Mercury from Mine Waste Calcine Using Simulated Human Body Fluids

OpenAIRE

Gray, John E.; Plumlee, Geoffrey S.; Morman, Suzette A.; Higueras, Pablo L.; Crock, James G.; Lowers, Heather A.; Witten, Mark L.

2010-01-01

In vitro bioaccessibility (IVBA) studies were carried out on samples of mercury (Hg) mine-waste calcine (roasted Hg ore) by leaching with simulated human body fluids. The objective was to estimate potential human exposure to Hg due to inhalation of airborne calcine particulates and hand-to-mouth ingestion of Hg-bearing calcines. Mine waste calcines collected from Hg mines at Almad?n, Spain, and Terlingua, Texas, contain Hg sulfide, elemental Hg, and soluble Hg compounds, which constitute prim...

Capture of Tritium Released from Cladding in the Zirconium Recycle Process

Energy Technology Data Exchange (ETDEWEB)

Spencer, Barry B [ORNL; Bruffey, Stephanie H [ORNL; DelCul, Guillermo Daniel [ORNL; Walker, Trenton Baird [ORNL

2016-08-31

Zirconium may be recovered from the Zircaloy® cladding of used nuclear fuel (UNF) for recycle or to reduce the quantities of high-level waste destined for a geologic repository. Recovery of zirconium using a chlorination process is currently under development at the Oak Ridge National Laboratory. The approach is to treat the cladding with chlorine gas to convert the zirconium in the alloy (~98 wt % of the alloy mass) to zirconium tetrachloride. A significant fraction of the tritium (0–96%) produced in nuclear fuel during irradiation may be found in zirconium-based cladding and could be released from the cladding when the solid matrix is destroyed by the chlorination reaction. To prevent uncontrolled release of radioactive tritium to other parts of the plant or to the environment, a method to recover the tritium may be required. The focus of this effort was to (1) identify potential methods for the recovery of tritium from the off-gas of the zirconium recycle process, (2) perform scoping tests on selected recovery methods using nonradioactive gas simulants, and (3) select a process design appropriate for testing on radioactive gas streams generated by the engineering-scale zirconium recycle demonstrations on radioactive used cladding.

Capture of Tritium Released from Cladding in the Zirconium Recycle Process

Energy Technology Data Exchange (ETDEWEB)

Bruffey, Stephanie H [ORNL; Spencer, Barry B [ORNL; DelCul, Guillermo Daniel [ORNL

2016-08-31

This report is issued as the first revision to FCRD-MRWFD-2016-000297. Zirconium may be recovered from the Zircaloy® cladding of used nuclear fuel (UNF) for recycle or to reduce the quantities of high-level waste destined for a geologic repository. Recovery of zirconium using a chlorination process is currently under development at the Oak Ridge National Laboratory. The approach is to treat the cladding with chlorine gas to convert the zirconium in the alloy (~98 wt % of the alloy mass) to zirconium tetrachloride. A significant fraction of the tritium (0–96%) produced in nuclear fuel during irradiation may be found in zirconium-based cladding and could be released from the cladding when the solid matrix is destroyed by the chlorination reaction. To prevent uncontrolled release of radioactive tritium to other parts of the plant or to the environment, a method to recover the tritium may be required. The focus of this effort was to (1) identify potential methods for the recovery of tritium from the off-gas of the zirconium recycle process, (2) perform scoping tests on selected recovery methods using non-radioactive gas simulants, and (3) select a process design appropriate for testing on radioactive gas streams generated by the engineering-scale zirconium recycle demonstrations on radioactive used cladding.

Corrosion resistant zirconium alloys prepared by powder metallurgy

International Nuclear Information System (INIS)

Wojeik, C.C.

1984-01-01

Pure zirconium and zirconium 2.5% niobium were prepared by powder metallurgy. The powders were prepared directly from sponge and consolidated by cold isostatic pressing and sintering. Hot isostatic pressing was also used to obtain full density after sintering. For pure zirconium the effects of particle size, compaction pressure, sintering temperature and purity were investigated. Fully densified zirconium and Zr-2.5%Nb exhibited tensile properties comparable to cast material at room temperature and 300 0 F (149 0 C). Pressed and sintered material having density of 94-99% had slightly lower tensile properties. Corrosion tests were performed in boiling 65% H/sub 2/SO/sub 4/, 70% HNO/sub 3/, 20% HCl and 20% HCl + 500 ppm FeCl/sub 3/ (a known pitting solution). For fully dense material the observed corrosion behavior was nearly equivalent to cast material. A slightly higher rate of attack was observed for samples which were only 94-99% dense. Welding tests were also performed on zirconium and Zr-2.5%Nb alloy. Unlike P/M titanium alloys, these materials had good weldability due to the lower content of volatile impurities in the powder. A slight amount of weld porosity was observed but joint efficiencies were always not 100%, even for 94-99% density samples. Several practical applications of the P/M processed material will be briefly described

Waste Calcining Facility remote inspection report

International Nuclear Information System (INIS)

Patterson, M.W.; Ison, W.M.

1994-08-01

The purpose of the Waste Calcining Facility (WCF) remote inspections was to evaluate areas in the facility which are difficult to access due to high radiation fields. The areas inspected were the ventilation exhaust duct, waste hold cell, adsorber manifold cell, off-gas cell, calciner cell and calciner vessel. The WCF solidified acidic, high-level mixed waste generated during nuclear fuel reprocessing. Solidification was accomplished through high temperature oxidation and evaporation. Since its shutdown in 1981, the WCFs vessels, piping systems, pumps, off-gas blowers and process cells have remained contaminated. Access to the below-grade areas is limited due to contamination and high radiation fields. Each inspection technique was tested with a mock-up in a radiologically clean area before the equipment was taken to the WCF for the actual inspection. During the inspections, essential information was obtained regarding the cleanliness, structural integrity, in-leakage of ground water, indications of process leaks, indications of corrosion, radiation levels and the general condition of the cells and equipment. In general, the cells contain a great deal of dust and debris, as well as hand tools, piping and miscellaneous equipment. Although the building appears to be structurally sound, the paint is peeling to some degree in all of the cells. Cracking and spalling of the concrete walls is evident in every cell, although the east wall of the off-gas cell is the worst. The results of the completed inspections and lessons learned will be used to plan future activities for stabilization and deactivation of the facility. Remote clean-up of loose piping, hand tools, and miscellaneous debris can start immediately while information from the inspections is factored into the conceptual design for deactivating the facility

Investigation on the corrosion resistance of zirconium in nitric acid

International Nuclear Information System (INIS)

Fauvet, P.; Mur, P.

1990-01-01

Zirconium in nitric solutions exhibits an excellent corrosion resistance in the passive state, and a mediocre corrosion resistance in the unpassive state with risk of stress corrosion cracking. Results of the influence of some parameters (medium, potential, temperature, stress, friction, metallurgical structure and surface state) on zirconium passivation are presented. Zirconium remains passive in a large range of HNO 3 concentration (at least up to 14.4N), in the presence of oxidizing ions (Cr 4 , Ce 4 ), in a spent fuel dissolution solution. Zirconium is depassived by friction at high speed and pressure, by platinum coupling in boiling 14.4N HNO 3 with or without stress, or by imposed deformation speed under high potential. (A.B.)

Thermotransport of nitrogen and oxygen in β-zirconium

NARCIS (Netherlands)

Vogel, D.L.; Rieck, G.D.

1971-01-01

An investigation of thermotransport of nitrogen in ß-zirconium is reported. Using a method previously described, the heat of transport turned out to be 25.1 kcal/mole with a standard deviation of 2.5 kcal/mole. The formerly published value of the heat of transport of oxygen in ß-zirconium, viz. 20

Fluidized bed system for calcination of high level radioactive waste

Energy Technology Data Exchange (ETDEWEB)

Pande, D P; Prasad, T L; Yadgiri, N K; Theyyunni, T K [Process Engineering and Systems Development Division, Bhabha Atomic Research Centre, Mumbai (India)

1994-06-01

During the operation of nuclear facilities significant quantities of radiochemical liquid effluents of different concentrations and varying chemical compositions are generated. These effluents contain activated radionuclides, corrosion products and fission products. The advantage of feeding the waste in solid form into the vitrifying equipment are multifold. Efforts are therefore made in many countries to calcine the high level waste, and obtain waste in the oxide form before the same is mixed with glass forming additives and fed into the melter unit. An experimental rig for fluidized bed calcination is constructed for carrying out the detailed investigation of this process, in order to adopt the same for plant scale application. To achieve better gas-solid contact and avoid raining down of solids, a distributor of bubble cap type was designed. A review of existing experience at various laboratories and design of new experimental facility for development of calciners are given. (author). 11 refs., 5 figs.

Dielectric properties of zirconium dioxide-based ceramics

International Nuclear Information System (INIS)

Vladimirova, O.S.; Gruzdev, A.I.; Koposova, Z.L.; Lyutsareva, L.A.

1985-01-01

This paper studies the dielectric properties of materials based on stabilized zirconium dioxide with Co 3 O 4 additions possessing a high temperature-coefficient of resistance. These materials are promising for manufacturing resistance temperature gages that work under an oxidizing atmosphere at 370-1270 degrees K. The obtained results indicate the possibility of developing temperature gases possessing highsensitivity from stabilized zirconium dioxide with Co 3 O 4 additions

METHOD OF IMPROVING CORROSION RESISTANCE OF ZIRCONIUM

Science.gov (United States)

Shannon, D.W.

1961-03-28

An improved intermediate rinse for zirconium counteracts an anomalous deposit that often results in crevices and outof-the-way places when ordinary water is used to rinse away a strong fluoride etching solution designed to promote passivation of the metal. The intermediate rinse, which is used after the etching solution and before the water, is characterized by a complexing agent for fluoride ions such as aluminum or zirconium nitrates or chlorides.

Accelerated irradiation growth of zirconium alloys

International Nuclear Information System (INIS)

Griffiths, M.; Gilbert, R.W.; Fidleris, V.

1989-01-01

This paper discusses how sponge zirconium and Zr-2.5 wt% Nb, Zircaloy, or Excel alloys all exhibit accelerated irradiation growth compared with high-purity crystal-bar zirconium for irradiation temperatures between 550 to 710 K and fluences between 0.1 to 10 x 10 25 n · m -2 (E > 1 MeV). There is generally an incubation period or fluence before the onset of accelerated or breakaway growth, which is dependent on the particular material being irradiated, its metallurgical condition before irradiation, and the irradiation temperature. Transmission electron microscopy has shown that there is a correlation between accelerated irradiation growth and the appearance of c-component vacancy loops on basal planes. Measurements in some specimens indicate that a significant fraction of the strain can be directly attributed to the loops themselves. There is considerable evidence to show that their formation is dependent both on the specimen purity and on the irradiation temperature. Materials that have a high interstitial-solute content contain c-component loops and exhibit high growth rates even at low fluences ( 2 :5 n · m -2 , E > 1 MeV). For sponge zirconium and the Zircaloys, c-component loop formation and the associated acceleration of growth (breakaway) during irradiation occurs because the intrinsic interstitial solute (mainly, oxygen, carbon and nitrogen) in the zirconium matrix is supplemented by interstitial iron, chromium, and nickel from the radiation-induced dissolution of precipitates. (author)

Primary Stability of Zirconium vs Titanium Implants: An In Vitro Comparison

Science.gov (United States)

2015-06-05

of any copyrighted material in the thesis manuscript entitled: Primary Stability of Zirconium vs Titanium Implants: An In Vitro Comparison Is...Uniformed Services University Date: 02/20/2015 Primary Stability of Zirconium vs Titanium Implants: An In Vitro Comparison By...the thesis manuscript entitled: Primary Stability of Zirconium vs Titanium Implants: An In Vitro Comparison Is appropriately acknowledged

Separation of zirconium from hafnium by ion exchange

Energy Technology Data Exchange (ETDEWEB)

Felipe, Elaine C.B.; Palhares, Hugo G.; Ladeira, Ana Claudia Q., E-mail: elainecfelipe@yahoo.com.br, E-mail: hugopalhares@gmail.com, E-mail: ana.ladeira@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

2013-07-01

Zirconium and hafnium are two of the most important metals for the nuclear industry. Hafnium occurs in all zirconium ores usually in the range 2 - 3%. However, for the most nuclear industry applications, it is necessary to use a zirconium of extremely pure level. The current work consists in the separation of zirconium and hafnium by the ion exchange method in order to obtain a zirconium concentrate of high purity. The zirconium and hafnium liquors were produced from the leaching of the Zr(OH){sub 4} and Hf(OH){sub 4} with nitric acid for 24 hours. From these two liquors it was prepared one solution containing 7.5 x 10{sup -2} mol L{sup -1} of Zr and 5.8 x 10{sup -3} mol L{sup -1} of Hf with acidity of 1 M. Ion exchange experiments were carried out in batch with the resins Dowex 50WX4, Dowex 50WX8 100, Dowex 50WX8 50, Amberlite IR-120 and Marathon C at constant temperature 28 deg C. Other variables such as, acidity and agitation were kept constant. The data were adjusted to Langmuir equation in order to calculate the maximum loading capacity (q{sub max}) of the resins, the distribution coefficient (K{sub d}) for Zr and Hf and the separation factor (α{sub Hf}{sup Zr} ). The results of maximum loading capacity (q{sub max}) for Zr and Hf, in mmol g{sup -}1, showed that the most suitable resins for columns experiments are: Dowex 50WX4 50 (q{sub max} Z{sub r} = 2.21, Hf = 0.18), Dowex 50WX8 50 (q{sub max} Zr = 1.89, Hf = 0.13) and Amberlite (q{sub max} Zr = 1.64, Hf = 0.12). However, separations factors, α{sub Hf}{sup Zr}, showed that the resins are not selective. (author)

Evaluation of Calcine Disposition Path Forward

International Nuclear Information System (INIS)

Birrer, S.A.; Heiser, M.B.

2003-01-01

This document describes an evaluation of the baseline and two alternative disposition paths for the final disposition of the calcine wastes stored at the Idaho Nuclear Technology and Engineering Center at the Idaho National Engineering and Environmental Laboratory. The pathways are evaluated against a prescribed set of criteria and a recommendation is made for the path forward

40 CFR 471.90 - Applicability; description of the zirconium-hafnium forming subcategory.

Science.gov (United States)

2010-07-01

... zirconium-hafnium forming subcategory. 471.90 Section 471.90 Protection of Environment ENVIRONMENTAL... POINT SOURCE CATEGORY Zirconium-Hafnium Forming Subcategory § 471.90 Applicability; description of the zirconium-hafnium forming subcategory. This subpart applies to discharges of pollutants to waters of the...

Development of Self-Healing Zirconium-Silicide Coatings for Improved Performance Zirconium-Alloy Fuel Cladding

Energy Technology Data Exchange (ETDEWEB)

Sridharan, Kumar [University of Wisconsin-Madison; Mariani, Robert [Idaho National Lab. (INL), Idaho Falls, ID (United States); Bai, Xianming [Idaho National Lab. (INL), Idaho Falls, ID (United States); Xu, Peng [Westinghouse Electric Company; Lahoda, Ed [Westinghouse Electric Company

2018-03-31

Given the long-term goal of developing such coatings for use with nuclear reactor fuel cladding, this work describes results of oxidation and corrosion behavior of bulk zirconium-silicide and fabrication of zirconium-silicide coatings on zirconium-alloy test flats, tube configurations, and SiC test flats. In addition, boiling heat transfer of these modified surfaces (including ZrSi2 coating) during clad quenching experiments is discussed in detail. Oxidation of bulk ZrSi2 was found to be negligible compared to Zircaloy-4 (a common Zr-alloy cladding material) and mechanical integrity of ZrSi2 was superior to that of bulk Zr2Si at high temperatures in ambient air. Very interesting and unique multi-nanolayered composite of ZrO2 and SiO2 were observed. Physical model for the oxidation has been proposed wherein Zr–Si–O mixture undergoes a spinodal phase decomposition into ZrO2 and SiO2, which is manifested as a nanoscale assembly of alternating layer of the two oxides. Steam corrosion at high pressure (10.3 MPa) led to weight loss of ZrSi2 and produced oxide scale with depletion of silicon, possibly attributed to volatile silicon hydroxide, gaseous silicon monoxide, and a solubility of silicon dioxide in water. Only Zircon phase (ZrSiO4) formed during oxidation of ZrSi2 at 1400°C in air, and allowed for immobilization silicon species in oxide scale in the aqueous environments. Zirconium-silicide coatings (on zirconium-alloy substrates) investigated in this study were deposited primarily using magnetron sputter deposition method and slurry method, although powder spray deposition processes cold spray and thermal spray methods were also investigated. The optimized ZrSi2 sputtered coating exhibited a highly protective nature at elevated temperatures in ambient air by mitigating oxygen permeation to the underlying zirconium alloy substrate. The high oxidation resistance of the coating has been shown to be due to nanocrystalline SiO2 and ZrSiO4 phases in the amorphous

Influence of zirconium ions on the sorption of carrier-free radiophosphate (32P)

International Nuclear Information System (INIS)

Friedmann, Ch.; Schoenfeld, T.

1975-01-01

In acid solutions the addition of zirconium ions largely affects the sorption of carrier-free radiophosphate on various materials. With some sorbents, such as diatomeceous earth, clay minerals or activated charcoal, the addition of small quantities of zirconium leads to a substantial increase of 32 P adsorption. On the other hand, important quantities of zirconium cause decrease of sorption. With alumina as an adsorbent, any addition of zirconium leads to reduced adsorption of radiophosphate. These phenomena are due to the formation of soluble zirconium-phosphate complex ions. (author)

Photometric determination of zirconium in phosphorites by reaction with arsenazo III

Energy Technology Data Exchange (ETDEWEB)

Nikol' skaya, I V; Maksimov, A V

1976-05-01

The reaction between zirconium and arsenazo III has been studied over a wide range of hydrochloric acid concentration and under different conditions. 6 and 9 M HCl solutions are optimal for determining zirconium; the least effect of phosphate ions and color stability in time are observed in this case. The determination of zirconium should be carried out using 10-fold reagent excess and in 15-20 min after adding the reagent. The interference of phosphate ions has been estimated. A procedure has been developed for photometric determination of zirconium in phosphorites with prior acid separation of soluble impurities.

Synthesis of well-dispersed ZnO nanomaterials by directly calcining zinc stearate

International Nuclear Information System (INIS)

Guo Guangsheng; Shi Chen; Tao Dongliang; Qian Weizhong; Han Dongmei

2009-01-01

Well-dispersed ZnO nanomaterials were synthesized by direct calcination of zinc stearate. Results from Fourier transform infrared (FT-IR) spectra and X-ray diffraction (XRD) indicated both the decomposition degree of organic ligand and the purity of calcined products were increased with the calcination temperature. The influence of decomposition temperature on the morphology of ZnO nanomaterials was investigated by field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The experimental results revealed the morphology of ZnO transformed from nanosheets to hexagonal nanopyramids and then to nanoparticles at 573, 673 and 773 K respectively. Finally, a morphology evolution model of ZnO nanomaterials under different temperatures was proposed

A half-century of changes in zirconium alloys

International Nuclear Information System (INIS)

Mardon, J.P.; Barberis, P.; Hoffmann, P.B.

2008-01-01

This article presents the history of zirconium alloys for PWR and BWR technologies. For more than 20 years zirconium alloys have evolved to cope with demands of the reactor operators concerning the burn-up extension and new safety margins. The poor properties of Zircaloy-1 concerning corrosion have led researchers to add elements like iron by developing Zircaloy-3A and Zircaloy-3C, and resulting in Zircaloy-4 with tin addition (from 1.30% to 1.50%). Zircaloy-4 is now outdated for PWR and new zirconium alloys with niobium are used (M5, ZIRLO...) they present a better resistance to corrosion, to hydridation, to creep and they are less prone to dimensional changes under irradiation. (A.C.)

Research and development of zirconium industry in China

International Nuclear Information System (INIS)

Liu Jianzhang; Tian Zhenye

2001-01-01

The development of uranium material for nuclear power and silicon material for information industry represents two revolutionary changes in the material field in 20-th century. The development of these kinds of materials not only brings about great revolution of technology in the material field, but also promotes the great advancement of the world economy. Zirconium or its alloy, as one of the most important material in atomic age, just as the same as foreign countries has been developed under promotion of nuclear submarine project in China, and building of civil nuclear power reactor then has been laid a solid foundation for zirconium industry and provide a broad market for zirconium material

The increase performance BMF-14 calcination unit

International Nuclear Information System (INIS)

Triyono

2013-01-01

The heating element of performance increase BMF-14 calcination unit has been installed. The activity includes: installation and function test heating element step by step. The main component includes: kanthal heating element type with size long 58,2 cm diameter 0,9 cm slot total 28, flexible cable resists heat 30 Amperes, band cable heat resists and flexible clamp. The heating elements installation includes from 3 groups and every groups have 4 heating elements to connectly series. Every group connecting to every phase RST and neutral for getting electric voltage 380 Volts follow contact relay 3 phases to controlling by digital temperature control. The resulting installation of heating element in the BMF-14 calcination unit showed that: BMF-14 calcination unit can be again of the setting temperature step by step. In the step I get optimal temperature 560 °C test time 1068 minutes with rate velocity heat 0 to 18,0 °C/minutes with current between 5,8 to 6,4 Amperes voltage 103 to 123 Volts (phase R and T). In the step II gets optimal temperature 600 °C test time 265 minutes getting rate velocity heat 0 to 40,3 °C/minutes with current 3,8 to 8,5 Amperes voltage 76 to 142 Volts (phase RST). In the step III gets optimal temperature 1000 °C test time 107 minutes getting rate velocity heat 0 to 53,5 °C/minutes with current 9,7 to 12,5 Amperes voltage 215 to 225 Volts (phase RST). (author)

Preparation of complexes of zirconium and hafnium tetrachlorides with phosphorus oxychloride

International Nuclear Information System (INIS)

Snyder, T.S.; Stoltz, R.A.

1989-01-01

This patent describes an improvement in a method for separating hafnium chloride from zirconium chloride using a distillation column, with a hafnium chloride enriched vapor stream taken from the top of the column and a zirconium enriched chloride stream taken from the bottom of the column. The improvement comprising: purifying the zirconium-hafnium chloride in a molten salt purification vessel prior to or after introduction into the distillation column to substantially eliminate iron chloride from the zirconium-hafnium chloride by at least periodically removing iron chloride from the molten salt purification vessel by electrochemically plating iron onto an electrode in the molten salt purification vessel. The molten salt in the molten salt purification vessel consisting essentially of a mixture of chlorides selected from the group consisting of alkali metals, alkaline earth metals, zirconium, hafnium, aluminum, manganese, and zinc

Zirconium distribution in the system HNO3-H2O-TBP-diluent

International Nuclear Information System (INIS)

Shu, J.; Araujo, B.F. de.

1984-01-01

The extraction behaviour of zirconium in TBP/diluent-HNO 3 -H 2 O systems is studied in order to increase the uranium decontamination factor by adjusting the extraction conditions so that zirconium extraction is kept at a minimum. Equilibrium diagram, TBP concentration, aqueous: organic phases ratio, salting-out effects and uranium loading in the organic phase were the main factors studied. All the experiments have been carried out with zirconium in the 10 -2 - 10 -3 M concentration range. The extractant degradation products influence upon zirconium behaviour was also verified. With the data obtained it was possible to introduce some modifications in the standard Purex flowsheet with the increase of the decontamination of uranium product from zirconium. (Author) [pt

Origin of Activity and Stability Enhancement for Ag3PO4 Photocatalyst after Calcination

Directory of Open Access Journals (Sweden)

Pengyu Dong

2016-11-01

Full Text Available Pristine Ag3PO4 microspheres were synthesized by a co-precipitation method, followed by being calcined at different temperatures to obtain a series of calcined Ag3PO4 photocatalysts. This work aims to investigate the origin of activity and stability enhancement for Ag3PO4 photocatalyst after calcination based on the systematical analyses of the structures, morphologies, chemical states of elements, oxygen defects, optical absorption properties, separation and transfer of photogenerated electron-hole pairs, and active species. The results indicate that oxygen vacancies (VO˙˙ are created and metallic silver nanoparticles (Ag NPs are formed by the reaction of partial Ag+ in Ag3PO4 semiconductor with the thermally excited electrons from Ag3PO4 and then deposited on the surface of Ag3PO4 microspheres during the calcination process. Among the calcined Ag3PO4 samples, the Ag3PO4-200 sample exhibits the best photocatalytic activity and greatly enhanced photocatalytic stability for photodegradation of methylene blue (MB solution under visible light irradiation. Oxygen vacancies play a significantly positive role in the enhancement of photocatalytic activity, while metallic Ag has a very important effect on improving the photocatalytic stability. Overall, the present work provides some powerful evidences and a deep understanding on the origin of activity and stability enhancement for the Ag3PO4 photocatalyst after calcination.

Sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides

Directory of Open Access Journals (Sweden)

R.V. Smotraiev

2016-05-01

Full Text Available The actual problem of water supply in the world and in Ukraine, in particular, is a high level of pollution in water resources and an insufficient level of drinking water purification. With industrial wastewater, a significant amount of pollutants falls into water bodies, including suspended particles, sulfates, iron compounds, heavy metals, etc. Aim: The aim of this work is to determine the impact of aluminum and manganese ions additives on surface and sorption properties of zirconium oxyhydroxide based sorbents during their production process. Materials and Methods: The sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides were prepared by sol-gel method during the hydrolysis of metal chlorides (zirconium oxychloride ZrOCl2, aluminum chloride AlCl3 and manganese chloride MnCl2 with carbamide. Results: The surface and sorption properties of sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides were investigated. X-ray amorphous structure and evolved hydroxyl-hydrate cover mainly characterize the obtained xerogels. The composite sorbents based on xerogels of zirconium oxyhydroxide doped with aluminum oxyhydroxide (aS = 537 m2/g and manganese oxyhydroxide (aS = 356 m2/g have more developed specific surface area than single-component xerogels of zirconium oxyhydroxide (aS = 236 m2/g and aluminum oxyhydroxide (aS = 327 m2/g. The sorbent based on the xerogel of zirconium and manganese oxyhydroxides have the maximum SO42--ions sorption capacity. It absorbs 1.5 times more SO42–-ions than the industrial anion exchanger AN-221. The sorbents based on xerogels of zirconium oxyhydroxide has the sorption capacity of Fe3+-ions that is 1.5…2 times greater than the capacity of the industrial cation exchanger KU-2-8. The Na+-ions absorption capacity is 1.47…1.56 mmol/g for each sorbent. Conclusions: Based on these data it can be concluded that the proposed method is effective for sorbents production based on

Model for the sulfidation of calcined limestone and its use in reactor models.

NARCIS (Netherlands)

Heesink, Albertus B.M.; Brilman, Derk Willem Frederik; van Swaaij, Willibrordus Petrus Maria

1998-01-01

A mathematical model describing the sulfidation of a single calcined limestone particle was developed and experimentally verified. This model, which includes no fitting parameters, assumes a calcined limestone particle to consist of spherical grains of various sizes that react with H2S according to

Manufacturing process to reduce large grain growth in zirconium alloys

International Nuclear Information System (INIS)

Rosecrans, P.M.

1987-01-01

A method is described of treating cold worked zirconium alloys to reduce large grain growth during thermal treatment above its recrystallization temperature. The method comprises heating the zirconium alloy at a temperature of about 1300 0 F. to 1350 0 F. for about 1 to 3 hours subsequent to cold working the zirconium alloy and prior to the thermal treatment at a temperature of between 1450 0 -1550 0 F., the thermal treatment temperature being above the recrystallization temperature

Method of purifying zirconium tetrachloride and hafnium tetrachloride in a vapor stream

International Nuclear Information System (INIS)

Snyder, T.S.; Stolz, R.A.

1992-01-01

This patent describes a method of purifying zirconium tetrachloride and hafnium tetrachloride in a vapor stream from a sand chlorinator in which the silicon and metals present in sand fed to the chlorinator are converted to chlorides at temperatures over about 800 degrees C. It comprises cooling a vapor stream from a sand chlorinator, the vapor stream containing principally silicon tetrachloride, zirconium tetrachloride, and hafnium tetrachloride contaminated with ferric chloride, to a temperature of from about 335 degrees C to about 600 degrees C; flowing the vapor stream through a gaseous diffusion separative barrier to produce a silicon tetrachloride-containing vapor stream concentrated in zirconium tetrachloride and hafnium tetrachloride and a silicon tetrachloride-containing vapor stream depleted in zirconium tetrachloride and hafnium tetrachloride; adsorbing the ferric chloride in the separative barrier; and recovering the silicon tetrachloride stream concentrated in zirconium tetrachloride and hafnium tetrachloride separately from the silicon tetrachloride stream depleted in zirconium tetrachloride and hafnium tetrachloride

Formation and dissolution of the anodic oxide film on zirconium in alcoholic aqueous solutions

International Nuclear Information System (INIS)

Mogoda, A.S.

1995-01-01

The dissolution behavior of the anodic oxide film formed in alcoholic aqueous solutions was studied. Results indicated the dissolution mechanism of the duplex oxide film followed a zero-order rate equation. The increase in methanol concentration in the formation medium (phosphoric acid [H 3 PO 4 ]) resulted in formation of an oxide film that incorporated little phosphate ion and that dissolved at a low rate. The dissolution rate of the oxide film decreased with increasing methanol concentration in the dissolution medium. This was attributed to the increase in the viscosity of the medium, which led to a decrease in the diffusion coefficient of the dissolution product of the zirconium oxide film. Dissolution of the anodic oxide film also was investigated as a function of the chain length of alcohols

An Assessment of Using Vibrational Compaction of Calcined HLW and LLW in DWPF Canisters

International Nuclear Information System (INIS)

Yi, Yun-Bo; Amme, Robert C.; Shayer, Zeev

2008-01-01

Since 1963, the INEL has calcined almost 8 million gallons of liquid mixed waste and liquid high-level waste, converting it to some 1.1 million gallons of dry calcine (about 4275.0 m3), which consists of alumina-and zirconia-based calcine and zirconia-sodium blend calcine. In addition, if all existing and projected future liquid wastes are solidified, approximately 2,000 m3 of additional calcine will be produced primarily from sodium-bearing waste. Calcine is a more desirable material to store than liquid radioactive waste because it reduces volume, is much less corrosive, less chemically reactive, less mobile under most conditions, easier to monitor and more protective of human health and the environment. This paper describes the technical issue involved in the development of a feasible solution for further volume reduction of calcined nuclear waste for transportation and long term storage, using a standard DWPF canister. This will be accomplished by developing a process wherein the canisters are transported into a vibrational machine, for further volume reduction by about 35%. The random compaction experiments show that this volume reduction is achievable. The main goal of this paper is to demonstrate through computer modeling that it is feasible to use volume reduction vibrational machine without developing stress/strain forces that will weaken the canister integrity. Specifically, the paper presents preliminary results of the stress/strain analysis of the DWPF canister as a function of granular calcined height during the compaction and verifying that the integrity of the canister is not compromised. This preliminary study will lead to the development of better technology for safe compactions of nuclear waste that will have significant economical impact on nuclear waste storage and treatment. The preliminary results will guide us to find better solutions to the following questions: 1) What are the optimum locations and directions (vertical versus horizontal or

Low stress creep behaviour of zirconium

International Nuclear Information System (INIS)

Prasad, N.

1989-01-01

Creep behaviour of alpha zirconium of grain size varying between 16 and 55 μm has been investigated in the temperature range 813 to 1003K at stresses upto 5.5 MNm -2 using high sensitive spring specimen geometry. Creep experiments on specimens of 50 μm grain size revealed a transition from lattice diffusion controlled viscous creep at temperatures greater than 940K to grain boundary diffusion controlled viscous creep at lower temperatures. Tests conducted on either side of the transition suggest the dominance of Nabarro-Herring and Coble creep processes respectively. Evidence for power-law creep has been observed in practically all the creep tests. Based on the experimental data obtained in the present study and those recently reported by Novotny et al (1985), Langdon creep mechanism maps have bee n constructed at 873 and 973K. With the help of these maps for zirconium and those published for titanium the low stress creep behaviour of zirconium and titanium are compared. (author). 22 refs., 11 figs., 3 tabs

Reaction between Hydrogen Sulfide and Limestone Calcines

Czech Academy of Sciences Publication Activity Database

Hartman, Miloslav; Svoboda, Karel; Trnka, Otakar; Čermák, Jiří

2002-01-01

Roč. 41, č. 10 (2002), s. 2392-2398 ISSN 0888-5885 R&D Projects: GA AV ČR IAA4072711; GA AV ČR IAA4072801 Keywords : hydrogen sulfide * limestone calcines * desulfurization Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 1.247, year: 2002

Electrocnecical behaviour of zirconium during its anodic polarization in nitrate solutions

International Nuclear Information System (INIS)

Stabrovskij, A.I.; Karasev, A.F.

1983-01-01

Electrochemical behaviour of zirconium during its anodic polarization in nitrate solutions is investigated in detail to find the method of its complete dissolution. A study has been made of the influence of varioUs factors: current density electric potential, composition and temperature of the solution, anodic polarization duration on the Zr anodic polarization in nitric acid, on the maximum permissible current density and on the zirconium yield to the solution. The zirconium polarization decreases with an acid concentration and temperature increase and increases with the current density. Iron nitrate additions to nitric acid decrease, while ammonium fluoride additions increase zirconium yield into the solution

TPE/REE separation with the use of zirconium salt of HDBP

Science.gov (United States)

Glekov, R. G.; Shmidt, O. V.; Palenik, Yu. V.; Goletsky, N. D.; Sukhareva, S. Yu.; Fedorov, Yu. S.; Zilberman, B. Ya.

2003-01-01

Partitioning of long-lived radionuclides (minor actinides, fission products) is considered as TBP-compatible ZEALEX-process for extraction separation of transplutonium elements (TPE) and rare-earth elements (REE), as well as Y, Mo, Fe and residual amounts of Np, Pu, U. Zirconium salt of dibutyl phosphoric acid (ZS-HDBP) dissolved in 30 % TBP is used as a solvent. The process was tested in multistage centrifugal contactors. Lanthanides, Y and TPE, as well as Mo, Fe were extracted from high-level Purex raffinate, Am and ceric subgroup of REE being separated from the polyvalent elements by stripping with HNO3. TPE/REE partitioning was achieved in the second cycle of the ZEALEX-process using DTPA in formic acid media. The integral decontamination factor of Am from La and Ce after both cycles is >200, from Pr and Nd 20-30 and from Sm and Eu 3.6; REE strips in both cycles contained <0,1% of the initial amount of TPE.

Spectrofluorimetric determination of hafnium and zirconium with 3,7-dihydroxyflavone

Energy Technology Data Exchange (ETDEWEB)

Ito, Takushi; Suzuki, Osamu; Seuzuki, Tetsuo; Murata, Akira

1986-04-01

The absorptive and fluorescent characteristics of the hafnium and zirconium complexes of 3-hydroxyflavone and its 12 hydroxy and methoxy derivatives have been studied. The fluorescence of the 1:1 hafnium - 3,7-dihydroxyflavone complex (lambdasub(ex.)397 nm,lambdasub(em.) 465 nm) in 3 M hydrochloric acid has been used to determine 2-40 ng ml/sup -1/ of hafnium. The fluorescence of the 1:1 zirconium - 3,7-dihydroxyflavone complex (lambdasub(ex.) 395 nm, lambda sub(em.) 465 nm) at pH 2.0 in 0.02 M sulphate solution has been used to determine 2-40 ng ml/sup -1/ of zirconium. These methods are very sensitive and can be used for the simultaneous determination of hafnium and zirconium with an error of about 5%.

Geologic structure of Gofitsky deposit of titanium and zirconium and perspectives of the reserve base of titanium and zirconium in Russia

Science.gov (United States)

Kukhmazov, Iskander

2016-04-01

With the fall of the Soviet Union, all the mining deposits of titanium and zirconium appeared outside of Russian Federation. Therefore the studying of deposits of titanium and zirconium in Russia is very important nowadays. There is a paradoxical situation in the country: in spite of possible existence of national mineral resource base of Ti-Zr material, which can cover needs of the country, Russia is the one of the largest buyers of imported Ti-Zr material in the world. Many deposits are not mined, and those which are in the process of mining have poor reserves. Demand for this raw material is very great not only for Russia, but also for the world in general. Today there is a scarcity of zircon around the world and it will only increase through time. Therefore prices of products of titanium and zirconium also increase. Consequently Russian deposits of titanium and zirconium with higher content than foreign may become competitive. Russia is forced to buy raw materials (zirconium and titanium production) from former Soviet Union countries at prices higher than the world's and thus incur huge losses, including customs charges. Russia should create its own mineral resource base of Ti-Zr. Studied titanium-zirconium deposits of Stavropol region may become the basis for the south part of Russia. At first, Beshpagirsky deposit should be pointed out. It has large reserves of ore sands with high content of Ti-Zr. A combination of favorable geographical position of the area with developed industrial infrastructure makes it very beneficial as an object for high priority development. Gofitsky deposit should be pointed out as well. Its sands have a wide areal distribution and a high content of titanium and zirconium. Chokrak, Karagan-Konksk and Sarmatian sediments of the Miocene of Gofitsky deposit are productive for titanium and zirconium placers within Stavropol region of Russia. Gofitsky deposit was evaluated from financial and economic point of view and the following data

Collaborative study of the colorimetric determination of zirconium in antiperspirant aerosols

International Nuclear Information System (INIS)

Beavin, P. Jr.

1977-01-01

A previously published method for determining zirconium in antiperspirant aerosols was collaboratively studied by 7 laboratories. The method consists of 2 procedures: a rapid dilution procedure for soluble zirconium compounds or a lengthier fusion procedure for total zirconium followed by colorimetric determination. The collaborators were asked to perform the following: Spiking materials representing 4 levels of soluble zirconium were added to weighed portions of a zirconium-free cream base concentrate and the portions were assayed by the dilution procedure. Spiking materials representing 4 levels of zirconium in either the soluble or the insoluble form (or as a mixture) were also added to portions of the same concentrate and these portions were assayed by the fusion procedure. They were also asked to concentrate and assay, by both procedures, 2 cans each of 2 commercial aerosol antiperspirants containing zirconyl hydroxychloride. The average percent recoveries and standard deviations for spiked samples were 99.8-100.2 and 1.69-2.71, respectively, for soluble compounds determined by the dilution procedure, and 93.8-97.4 and 3.09-4.78, respectively, for soluble and/or insoluble compounds determined by the fusion procedure. The average perent zirconium found by the dilution procedure in the 2 commercial aerosol products was 0.751 and 0.792. Insufficient collaborative results were received for the fusion procedure for statistical evaluation. The dilution procedure has been adopted as official first action

Hydrogen outbreak of Zirconium Molybdate Hihydrate

International Nuclear Information System (INIS)

Miura, Yasuhiko; Fukuda, Kazuhiro; Ochi, Eiji

2008-01-01

JNFL is planning to construct a facility for enclosing the hull and end pieces produced due to reprocessing of spent fuel into stainless canisters after compressing, while those hull and end pieces enclosed into the stainless canisters are called 'compressed hulls'. Since the compressed hulls contain moisture absorbent Zirconium Molybdate Hihydrate accompanying hull and end pieces, there is a risk of outbreak of radiolysisradiolysis gas such as hydrogen, etc. by radiolysisradiolysis. This report intends to state the result of radiation irradiation experiment with the purpose of examining the volume of hydrogen outbreak from Zirconium Molybdate Hihydrate of the compressed hulls. (author)

Electron microscopy of nuclear zirconium alloys

International Nuclear Information System (INIS)

Versaci, R.A.; Ipohorski, Miguel

1986-01-01

Transmission electron microscopy observations of the microstructure of zirconium alloys used in fuel sheaths of nuclear power reactors are reported. Specimens were observed after different thermal and mechanical treatment, similar to those actually used during fabrication of the sheaths. Electron micrographs and electron diffraction patterns of second phase particles present in zircaloy-2 and zircaloy-4 were also obtained, as well as some characteristic parameters. Images of oxides and hydrides most commonly present in zirconium alloys are also shown. Finally, the structure of a Zr-2,5Nb alloy used in CANDU reactors pressure tubes, is observed by electron microscopy. (Author) [es

Influence of starting precursors and synthesis methods on the physiochemical properties of zirconia

Energy Technology Data Exchange (ETDEWEB)

Gaydhankar, T.R., E-mail: tr.gaydhankar@ncl.res.in [Catalysis Division, National Chemical Laboratory, Pune 411008 (India); Jha, R.K. [Catalysis Division, National Chemical Laboratory, Pune 411008 (India); Nikalje, M.D. [Department of Chemistry, University of Pune, Pune 411 007 (India); Waghmare, K.J. [Catalysis Division, National Chemical Laboratory, Pune 411008 (India)

2014-07-01

Graphical abstract: Crystallite size of tetragonal phase of the zirconia samples prepared using different synthesis parameters and precursors as a function of calcination temperature. Surface area values of the zirconia samples calcined at 500 and 700 °C are in given brackets. - Highlights: • Zirconia prepared with modified sol–gel method is less stable compared with zirconia prepared by precipitation method. • Optimized synthesis conditions shifted the glow exotherm to higher temperature range indicating better thermal stability. • Tetragonal-zirconia could be synthesized in cost-effective manner using zirconium oxy-nitrate. • In our studies no co-relation between the surface area and crystallite size was observed. - Abstract: Under identical and judiciously pre-optimized synthesis conditions, the influence of different combinations of zirconium sources and/or post treatment conditions on structural properties, thermal stability, phase composition and morphology of zirconia has been investigated. High surface area tetragonal zirconia could be synthesized in a cost-effective manner from 1 M solution of zirconium oxy-nitrate at pH 11 using aqueous ammonia solution as a precipitant when calcined at 400 °C for 3 h. Irrespective of the preparation method, pH and starting precursor, zirconia samples prepared without digestion contained dominant monoclinic phase with some traces of tetragonal phase when calcined at 700 °C. Even though there is linear decrease in surface area with increase in the crystallite size for each sample as a function of calcination temperature, no co-relation between the surface area and crystallite size could be achieved. SEM images show agglomerated and irregular shape particles between 10 to 20 μm.

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

International Nuclear Information System (INIS)

Takashima, Kyoichiro; Toida, Yukio

1994-01-01

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

A review of the inorganic and organometallic chemistry of zirconium

International Nuclear Information System (INIS)

Kalvins, A.K.

1985-01-01

The results of a literature review of the inorganic and organometallic chemistry of zirconium are presented. Compounds with physical and chemical properties compatible with the requirements of an ir laser zirconium isotope separation process have been identified

Mechanical resistance of zirconium implant abutments: A review of the literature

Science.gov (United States)

Vaquero-Aguilar, Cristina; Torres-Lagares, Daniel; Jiménez-Melendo, Manuel; Gutiérrez-Pérez, José L.

2012-01-01

The increase of aesthetic demands, together with the successful outcome of current implants, has renewed interest in the search for new materials with enough mechanical properties and better aesthetic qualities than the materials customarily used in implanto-prosthetic rehabilitation. Among these materials, zirconium has been used in different types of implants, including prosthetic abutments. The aim of the present review is to analyse current scientific evidence supporting the use of this material for the above mentioned purposes. We carried out the review of the literature published in the last ten years (2000 through 2010) of in vitro trials of dynamic and static loading of zirconium abutments found in the databases of Medline and Cochrane using the key words zirconium abutment, fracture resistance, fracture strength, cyclic loading. Although we have found a wide variability of values among the different studies, abutments show favourable clinical behaviour for the rehabilitation of single implants in the anterior area. Such variability may be explained by the difficulty to simulate daily mastication under in vitro conditions. The clinical evidence, as found in our study, does not recommend the use of implanto-prosthetic zirconium abutments in the molar area. Key words: Zirconium abutment, zirconium implant abutment, zirconia abutment, fracture resistance, fracture strength, cyclic loading. PMID:22143702

Synthesis, Characterization and Antimicrobial Activity of Zirconium (IV) Complexes

Energy Technology Data Exchange (ETDEWEB)

Sharma, Shobhana; Jain, Asha; Saxena, Sanjiv [Univ. of Rajasthan, Jaipur (India)

2012-08-15

Heteroleptic complexes of zirconium (IV) derived from bulky Schiff base ligands containing a sulphur atom and oximes of heterocyclic β-diketones of the general formula ZrLL' (where L'H{sub 2}=RCNH(C{sub 6}H{sub 4})SC : C(OH)N(C{sub 6}H{sub 5})N : CCH{sub 3}, R=-C{sub 6}H{sub 5}, -C{sub 6}H{sub 4}Cl(p) and L'H{sub 2}=R'C : (NOH)C : C(OH)N(C{sub 6}H{sub 5})N : CCH{sub 3}, R' = -CH{sub 2}CH{sub 3}, -C{sub 6}H{sub 5}, -C{sub 6}H{sub 4}Cl (p) were prepared by the reactions of zirconium tetrachloride with disodium salts of Schiff bases (L Na{sub 2}) and oximes of heterocyclic β-diketones (L' Na{sub 2}) in 1:1:1 molar ratio in dry refluxing THF. The structures of these monomeric zirconium (IV) complexes were elucidated with the help of elemental analysis, molecular weight measurements, spectroscopic (IR, NMR and mass) studies. A distorted trigonal bipyramidal geometry may be suggested for these heteroleptic zirconium (IV) complexes. The ligands (bulky Schiff base ligands containing a sulphur atom and oximes of heterocyclic β-diketones) and their heteroleptic complexes of zirconium (IV) were screened against A. flavus, P. aeruginesa and E. coli.

40 CFR 421.330 - Applicability: Description of the primary zirconium and hafnium subcategory.

Science.gov (United States)

2010-07-01

... primary zirconium and hafnium subcategory. 421.330 Section 421.330 Protection of Environment ENVIRONMENTAL... CATEGORY Primary Zirconium and Hafnium Subcategory § 421.330 Applicability: Description of the primary zirconium and hafnium subcategory. The provisions of this subpart are applicable to discharges resulting...

Historical fuel reprocessing and HLW management in Idaho

International Nuclear Information System (INIS)

Knecht, D.A.; Staiger, M.D.; Christian, J.D.

1997-01-01

This article review some of the key decision points in the historical development of spent fuel reprocessing and waste management practices at the Idaho Chemical Processing Plant that have helped ICPP to successfully accomplish its mission safely and with minimal impact on the environment. Topics include ICPP reprocessing development; batch aluminum-uranium dissolution; continuous aluminum uranium dissolution; batch zirconium dissolution; batch stainless steel dissolution; semicontinuous zirconium dissolution with soluble poison; electrolytic dissolution of stainless steel-clad fuel; graphite-based rover fuel processing; fluorinel fuel processing; ICPP waste management consideration and design decisions; calcination technology development; ICPP calcination demonstration and hot operations; NWCF design, construction, and operation; HLW immobilization technology development. 80 refs., 4 figs

Laves intermetallics in stainless steel-zirconium alloys

International Nuclear Information System (INIS)

Abraham, D.P.; McDeavitt, S.M.; Richardson, J.W. Jr.

1997-01-01

Laves intermetallics have a significant effect on properties of metal waste forms being developed at Argonne National Laboratory. These waste forms are stainless steel-zirconium alloys that will contain radioactive metal isotopes isolated from spent nuclear fuel by electrometallurgical treatment. The baseline waste form composition for stainless steel-clad fuels is stainless steel-15 wt.% zirconium (SS-15Zr). This article presents results of neutron diffraction measurements, heat-treatment studies and mechanical testing on SS-15Zr alloys. The Laves intermetallics in these alloys, labeled Zr(Fe,Cr,Ni) 2+x , have both C36 and C15 crystal structures. A fraction of these intermetallics transform into (Fe,Cr,Ni) 23 Zr 6 during high-temperature annealing; the authors have proposed a mechanism for this transformation. The SS-15Zr alloys show virtually no elongation in uniaxial tension, but exhibit good strength and ductility in compression tests. This article also presents neutron diffraction and microstructural data for a stainless steel-42 wt.% zirconium (SS-42Zr) alloy

Interrelationship between structure and corrosion behaviour of zirconium

Energy Technology Data Exchange (ETDEWEB)

Guenther, T [Bayer A.G., Leverkusen (Germany, F.R.)

1979-05-01

Due to plant failures caused by the break-down of zirconium grade 702 subjected to sulphuric acid the structure and corrosion behaviour of welded and as delivered specimens were tested for various heat treatments. It was shown by structure investigations and electron microprobe analysis that the corrosion behaviour of zirconium (in boiling 65 pct sulphuric acid) is strongly infuenced by the structure, which in its turn is dependent on the grade of purity and the prehistory of the material. Type, amount, and distribution of residual elements or precipitations caused by them are responsible for the corrosion resistance. This is valid particularly for the element iron. The plant failures mentioned here coincided with the examination results. Measures to improve the chemical resistance of pure zirconium subjected to extremely aggressive media were derived.

The flashcal process for the fabrication of fuel-metal oxides using the whiteshell roto-spray calciner

International Nuclear Information System (INIS)

Sridhar, T.S.

1988-01-01

A one-step, continuous, thermochemical calcination process, called the FLASHCAL (Flash Calcination) process has been developed for the production of single- and mixed-oxide powders of fuel metals (uranium, thorium and plutonium) from the respective nitrate solutions using the Whiteshell Roto-Spray Calciner (RSC). The metal-nitrate feed solution, either by itself or mixed with a suitable chemical reactant or additive, is converted to its oxide powder in the RSC at temperatures between 300 and 600 0 C. Rapid denitration takes place in the calciner, yielding the metal-oxide powders while simultaneously destroying any excess chemical additive and reaction by-products. In the production of precursor oxide powders suitable for fuel fabrication, the FLASHCAL process has advantages over batch calcination and other processes that involve precipitation and filtration steps because fewer processing and handling operations are needed. Results obtained with thorium nitrate and uranium nitrate-thorium nitrate mixtures indicate that some measure of control over the size distribution and morphology of the oxide product powders is possible in this process with the proper selection of chemical additive, as well as the operating parameters of the calciner

Design criteria for the new waste calcining facility at the Idaho Chemical Processing Plant

International Nuclear Information System (INIS)

Anderson, F.H.; Bingham, G.E.; Buckham, J.A.; Dickey, B.R.; Slansky, C.M.; Wheeler, B.R.

1976-01-01

The New Waste Calcining Facility (NWCF) at the Idaho Chemical Processing Plant (ICPP) is being built to replace the existing fluidized-bed, high-level waste calcining facility (WCF). Performance of the WCF is reviewed, equipment failures in WCF operation are examined, and pilot-plant studies on calciner improvements are given in relation to NWCF design. Design features of the NWCF are given with emphasis on process and equipment improvements. A major feature of the NWCF is the use of remote maintenance facilities for equipment with high maintenance requirements, thereby reducing personnel exposures during maintenance and reducing downtime resulting from plant decontamination. The NWCF will have a design net processing rate of 11.36 m 3 of high-level waste per day, and will incorporate in-bed combustion of kerosene for heating the fluidized bed calciner. The off-gas cleaning system will be similar to that for the WCF

A conceptual and calculational model for gas formation from impure calcined plutonium oxides

International Nuclear Information System (INIS)

Lyman, John L.; Eller, P. Gary

2000-01-01

Safe transport and storage of pure and impure plutonium oxides requires an understanding of processes that may generate or consume gases in a confined storage vessel. We have formulated conceptual and calculational models for gas formation from calcined materials. The conceptual model for impure calcined plutonium oxides is based on the data collected to date

The leaching of base minerals from the calcines produced by the roasting of pyrite concentrates

International Nuclear Information System (INIS)

Nicol, M.J.; Filmer, A.O.

1985-01-01

A number of gold and uranium plants in South Africa concentrate the pyrite in the ore residue by flotation and roast the concentrate for the production of sulphuric acid. The calcine produced, which is predominantly hematite, is generally subjected to cyanidation for the recovery of gold and silver. The calcines often contain economically significant quantities of copper, nickel , cobalt and uranium. Prior treatment of the calcine for the recovery of these metals would be desirable in terms of the value of the products. Several processes for the leaching of the base metals from plant calcines have been investigated, and an important general conclusion is that an adequate recovery of the base metals requires that a large proportion of the iron should also be extracted. This observation led to a more extensive investigation of the kinetics of leaching of various iron oxides. The application of electrochemical theory and techniques resulted in a fuller understanding of the various factors that govern the rate of leaching of iron oxides. As a result of this fundamental work, alternative treatment schemes that should yield more efficient extraction from calcines were suggested. Several of these possibilities were investigated, and the most promising were found to require reducing conditions during the leach, or prior partial reduction of the calcine to magnetite or wustite

Identification and characterization of a new Zirconium hydride

International Nuclear Information System (INIS)

Zhao, Z.

2007-01-01

In order to control the integrity of the fuel clad, alloy of zirconium, it is necessary to predict the behavior of zirconium hydrides in the environment (temperature, stress...), at a microscopic scale. A characterization study by TEM of hydrides has been realized. It shows little hydrides about 500 nm, in hydride Zircaloy 4. Then a more detailed study identified a new hydride phase presented in this paper. (A.L.B.)

Sorption of cesium on titanium and zirconium phosphates

International Nuclear Information System (INIS)

Lebedev, V.N.; Mel'nik, N.A.; Rudenko, A.V.

2003-01-01

Titanium and zirconium phosphates were prepared from mineral raw materials of the Kola Peninsula. Their capability to recover cesium cations from the model solutions and liquid radioactive waste (LRW) was studied. Titanium phosphate prepared from solutions formed by titanite breakdown demonstrates greater distribution coefficients of cesium as compared to zirconium phosphate. Titanium phosphate as a cheaper agent featuring greater sorption capacity was recommended for treatment of LRW to remove cesium [ru

[The clinical application of zirconium-dioxide-ceramics. Case report].

Science.gov (United States)

Somfai, Dóra; Zsigmond, Ágnes; Károlyházy, Katalin; Kispély, Barbara; Hermann, Péter

2015-12-01

Due to its outstanding physical, mechanical and esthetic properties, zirconium-dioxide is one of the most popular non-metal denture, capable of surpassing PFM in most cases. The recent advances of CAD/CAM technology makes it a good alternitve. Here we show the usefulness of zirconium-dioxide in everyday dental practice through three case reports.

Peculiarities of formation of zirconium aluminides in hydride cycle mode

International Nuclear Information System (INIS)

Muradyan, G.N.

2016-01-01

The zirconium aluminides are promising structural materials in aerospace, mechanical engineering, chemical industry, etc. They are promising for manufacturing of heat-resistant wires, that will improve the reliability and efficiency of electrical networks. In the present work, the results of study of zirconium aluminides formation in the Hydride Cycle (HC) mode, developed in the Laboratory of high-temperature synthesis of the Institute of Chemical Physics of NAS RA, are described. The formation of zirconium aluminides in HC proceeded according to the reaction xZrH_2+(1-x)Al → alloy Zr_xAl(1-x)+H_2↑. The samples were certified using: chemical analysis to determine the content of hydrogen (pyrolysis method); differential thermal analysis (DTA, derivatograph Q-1500, T_heating = 1000°C, rate 20°C/min); X-ray analysis (XRD, diffractometer DRON-0.5). The influences of the ratio of powders ZrH_2/Al in the reaction mixture, compacting pressure, temperature and heating velocity on the characteristics of the synthesized aluminides were determined. In HC, the solid solutions of Al in Zr, single phase ZrAl_2 and ZrAl_3 aluminides and Zr_3AlH_4.49 hydride were synthesized. Formation of aluminides in HC mode took place by the solid-phase mechanism, without melting of aluminum. During processing, the heating of the initial charge up to 540°C resulted in the decomposition of zirconium hydride (ZrH_2) to HCC ZrH_1.5, that interacted with aluminum at 630°C forming FCC alumohydride of zirconium. Further increase of the temperature up to 800°C led to complete decomposition of the formed alumohydride of zirconium. The final formation of the zirconium aluminide occurred at 1000-1100°C in the end of HC process. Conclusion: in the synthesis of zirconium aluminides, the HC mode has several significant advantages over the conventional modes: lower operating temperatures (1000°C instead of 1800°C); shorter duration (1.5-2 hours instead of tens of hours); the availability of

Distribution of zirconium in the nitric acid-water-TPB-diluent system

International Nuclear Information System (INIS)

Shu, J.; Floh de Araujo, B.

1984-10-01

This paper deals with the extraction behaviour of zirconium in TBP/diluent-HNO 3 -H 2 O systems. The main purpose is to increase the uranium decontamination factor by adjusting the extraction conditions so that zirconium extraction is kept at a mininum. Equilibrium diagram, TBP concentration, aqueous: organic phases ratio, salting-out effects and uranium loading in the organic phase were the main factors studied. All the experiments have been carried out with zirconium in the 10 -2 - 10 -3 M concentration range. The extractant degradation products influence upon ziconium behaviour was also verified. With the data obtained it was possible to introduce some modification in the standard Purex flow-sheet with the increase of the decontamination of uranium from zirconium. 5 refs., 9 figs

Comparison of Zirconium Phosphonate-Modified Surfaces for Immobilizing Phosphopeptides and Phosphate-Tagged Proteins.

Science.gov (United States)

Forato, Florian; Liu, Hao; Benoit, Roland; Fayon, Franck; Charlier, Cathy; Fateh, Amina; Defontaine, Alain; Tellier, Charles; Talham, Daniel R; Queffélec, Clémence; Bujoli, Bruno

2016-06-07

Different routes for preparing zirconium phosphonate-modified surfaces for immobilizing biomolecular probes are compared. Two chemical-modification approaches were explored to form self-assembled monolayers on commercially available primary amine-functionalized slides, and the resulting surfaces were compared to well-characterized zirconium phosphonate monolayer-modified supports prepared using Langmuir-Blodgett methods. When using POCl3 as the amine phosphorylating agent followed by treatment with zirconyl chloride, the result was not a zirconium-phosphonate monolayer, as commonly assumed in the literature, but rather the process gives adsorbed zirconium oxide/hydroxide species and to a lower extent adsorbed zirconium phosphate and/or phosphonate. Reactions giving rise to these products were modeled in homogeneous-phase studies. Nevertheless, each of the three modified surfaces effectively immobilized phosphopeptides and phosphopeptide tags fused to an affinity protein. Unexpectedly, the zirconium oxide/hydroxide modified surface, formed by treating the amine-coated slides with POCl3/Zr(4+), afforded better immobilization of the peptides and proteins and efficient capture of their targets.

Separation process of zirconium and hafnium

International Nuclear Information System (INIS)

Hure, J.; Saint-James, R.

1955-01-01

About the separation different processes of zirconium-hafnium, the extraction by solvent in cross-current is the most easily the process usable on an industrial scale. It uses tributyl phosphate as solvent, diluted with white spirit to facilitate the decanting. Some exploratory tests showed that nitric environment seemed the most favorable for extraction; but a lot of other factors intervene in the separation process. We studied the influence of the acidity successively, the NO 3 - ions concentration, the role of the cation coming with NO 3 - , as well as the influence of the concentration of zirconium in the solution on the separation coefficient β = α Zr / α Hf . (M.B.) [fr

Zirconium diselenite microstructures, formation and mechanism

Science.gov (United States)

Naik, Chandan C.; Salker, A. V.

2018-04-01

In this work, a series of microstructures of zirconium diselenite (Zr(SeO3)2) has been prepared via a simple precipitation method at room temperature without adding any organic surfactants. Phase purity of the sample has been checked by X-ray Diffraction. From the SEM, FESEM, and TEM images spheroid nanoparticles to the starfish-like structure of zirconium diselenite are detected. The morphological evolution processes were investigated carefully following time-dependent experiments and a growth mechanism has been proposed. Two different crystal growth processes, the oriented attachment process accompanying the Ostwald ripening process were held responsible for the formation of a structure resembling starfish having four arms.

A computer model for hydride blister growth in zirconium alloys

International Nuclear Information System (INIS)

White, A.J.; Sawatzky, A.; Woo, C.H.

1985-06-01

The failure of a Zircaloy-2 pressure tube in the Pickering unit 2 reactor started at a series of zirconium hydride blisters on the outside of the pressure tube. These blisters resulted from the thermal diffusion of hydrogen to the cooler regions of the pressure tube. In this report the physics of thermal diffusion of hydrogen in zirconium is reviewed and a computer model for blister growth in two-dimensional Cartesian geometry is described. The model is used to show that the blister-growth rate in a two-phase zirconium/zirconium-hydride region does not depend on the initial hydrogen concentration nor on the hydrogen pick-up rate, and that for a fixed far-field temperature there is an optimum pressure-type/calandria-tube contact temperature for growing blisters. The model described here can also be used to study large-scale effects, such as hydrogen-depletion zones around hydride blisters

Hydrogen content in titanium and a titanium–zirconium alloy after acid etching

Energy Technology Data Exchange (ETDEWEB)

Frank, Matthias J.; Walter, Martin S. [Department of Biomaterials, Institute for Clinical Dentistry, University of Oslo, P.O. Box 1109, Blindern, NO-0317 Oslo (Norway); Institute of Medical and Polymer Engineering, Chair of Medical Engineering, Technische Universität München, Boltzmannstrasse 15, 85748 Garching (Germany); Lyngstadaas, S. Petter [Department of Biomaterials, Institute for Clinical Dentistry, University of Oslo, P.O. Box 1109, Blindern, NO-0317 Oslo (Norway); Wintermantel, Erich [Institute of Medical and Polymer Engineering, Chair of Medical Engineering, Technische Universität München, Boltzmannstrasse 15, 85748 Garching (Germany); Haugen, Håvard J., E-mail: h.j.haugen@odont.uio.no [Department of Biomaterials, Institute for Clinical Dentistry, University of Oslo, P.O. Box 1109, Blindern, NO-0317 Oslo (Norway)

2013-04-01

Dental implant alloys made from titanium and zirconium are known for their high mechanical strength, fracture toughness and corrosion resistance in comparison with commercially pure titanium. The aim of the study was to investigate possible differences in the surface chemistry and/or surface topography of titanium and titanium–zirconium surfaces after sand blasting and acid etching. The two surfaces were compared by X-ray photoelectron spectroscopy, secondary ion mass spectroscopy, scanning electron microscopy and profilometry. The 1.9 times greater surface hydrogen concentration of titanium zirconium compared to titanium was found to be the major difference between the two materials. Zirconium appeared to enhance hydride formation on titanium alloys when etched in acid. Surface topography revealed significant differences on the micro and nanoscale. Surface roughness was increased significantly (p < 0.01) on the titanium–zirconium alloy. High-resolution images showed nanostructures only present on titanium zirconium. - Highlights: ► TiZr alloy showed increased hydrogen levels over Ti. ► The alloying element Zr appeared to catalyze hydrogen absorption in Ti. ► Surface roughness was significantly increased for the TiZr alloy over Ti. ► TiZr alloy revealed nanostructures not observed for Ti.

Ninth Processing Campaign in the Waste Calcining Facility

International Nuclear Information System (INIS)

Childs, K.F.; Donovan, R.I.; Swenson, M.C.

1982-04-01

This report discusses the Ninth (and final) Processing Campaign at the Waste Calcining Facility. Several processing interruptions were experienced during this campaign and the emphasis of this report is on process and equipment performance with operating problems and corrective actions discussed in detail

Zirconium-made equipment for the new La Hague reprocessing plants

International Nuclear Information System (INIS)

Decours, J.; Demay, R.; Bernard, C.; Mouroux, J.P.; Simonnet, J.

1991-01-01

The use of zirconium was developed to solve some problems of severe corrosion in boiling nitric medium, and to guarantee the service life of the equipment concerned. The paper presents the experience gained since the early 1970s, when the first units made of zirconium were used in French reprocessing plants. For the new La Hague UP3 and UP2 800 plants, it was decided to extend the use of zirconium to make large-scale equipment and, to do so, a major R and D program was implemented, of which the main results are presented

In-situ stabilization of radioactive zirconium swarf

Science.gov (United States)

Hess, Clay C.

1999-01-01

The method for treating ignitable cutting swarf in accordance with the present invention involves collecting cutting swarf in a casting mold underwater and injecting a binder mixture comprising vinyl ester styrene into the vessel to fill void volume; and form a mixture comprising swarf and vinyl ester styrene; and curing the mixture. The method is especially useful for stabilizing the ignitable characteristics of radioactive zirconium cutting swarf, and can be used to solidify zirconium swarf, or other ignitable finely divided material, underwater. The process could also be performed out of water with other particulate wastes.

Preparation of high-purity zirconium dioxide from baddeleyite

International Nuclear Information System (INIS)

Voskobojnikov, N.B.; Skiba, G.S.

1996-01-01

Interaction of baddeleyite concentrate with calcium oxide and calcium chloride in the process of caking is studied. The influence of grain size on calcium zirconate formation is tested. Conditions for cake leaching by hydrochloric acid and zirconium(4) oxychloride purification from calcium and silicon compounds by recrystallization are reported. Zirconium dioxide corresponding to specifications (6-2 special purity) is obtained with a high (more than 90%) chemical yield. 9 refs., 1 tab

Determination of the Rate of Formation of Hydroceramic Waste Forms made with INEEL Calcined Wastes

Energy Technology Data Exchange (ETDEWEB)

Barry Scheetz; Johnson Olanrewaju

2001-10-15

The formulation, synthesis, characterization and hydration kinetics of hydroceramic waste forms designed as potential hosts for existing INEEL calcine high-level wastes have been established as functions of temperature and processing time. Initial experimentations were conducted with several aluminosilicate pozzolanic materials, ranging from fly ash obtained from various power generating coal and other combustion industries to reactive alumina, natural clays and ground bottled glass powders. The final selection criteria were based on the ease of processing, excellent physical properties and chemical durability (low-leaching) determined from the PCT test produced in hydroceramic. The formulation contains vermiculite, Sr(NO32), CsC1, NaOH, thermally altered (calcined natural clay) and INEEL simulated calcine high-level nuclear wastes and 30 weight percent of fluorinel blend calcine and zirconia calcine. Syntheses were carried out at 75-200 degree C at autogeneous water pressure (100% relative humidity) at various time intervals. The resulting monolithic compact products were hard and resisted breaking when dropped from a 5 ft height. Hydroceramic host mixed with fluorinel blend calcine and processed at 75 degree C crumbled into rice hull-side grains or developed scaly flakes. However, the samples equally possessed the same chemical durability as their unbroken counterparts. Phase identification by XRD revealed that hydroceramic host crystallized type zeolite at 75-150 degree C and NaP1 at 175-200 degree C in addition to the presence of quartz phase originating from the clay reactant. Hydroceramic host mixed with either fluorinel blend calcine or zirconia calcine crystallized type A zeolite at 75-95 degree C, formed a mixture of type A zeolite and hydroxysodalite at 125-150 degree C and hydroxysodalite at 175-200 degree C. Quartz, calcium fluoride and zirconia phases from the clay reactant and the two calcine wastes were also detected. The PCT test solution

Effect of calcination routes on phase formation of BaTiO3 and their electronic and magnetic properties

Science.gov (United States)

Majumder, Supriyo; Choudhary, R. J.; Tripathi, M.; Phase, D. M.

2018-05-01

We have investigated the phase formation and correlation between electronic and magnetic properties of oxygen deficient BaTiO3 ceramics, synthesized by solid state reaction method, following different calcination paths. The phase analysis divulge that a higher calcination temperature above 1000° C is favored for tetragonal phase formation than the cubic phase. The core level X-ray photo electron spectroscopy measurements confirm the presence of oxygen vacancies and oxygen vacancy mediated Ti3+ states. As the calcination temperature and calcination time increases these oxygen vacancies and hence Ti3+ concentrations reduce in the sample. The temperature dependent magnetization curves suggest unexpected magnetic ordering, which may be due to the presence of unpaired electron at the t2g state (d1) of nearest-neighbor Ti atoms. In magnetization vs magnetic field isotherms, the regular decrease of saturation moment value with increasing calcination temperature and calcination time, can be discussed considering the amount of oxygen deficiency induced Ti3+ concentrations, present in the sample.

Concept Feasibility Report for Electroplating Zirconium onto Uranium Foil - Year 2

Energy Technology Data Exchange (ETDEWEB)

Coffey, Greg W. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Meinhardt, Kerry D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Joshi, Vineet V. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Pederson, Larry R. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Lavender, Curt A. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Burkes, Douglas [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

2015-03-01

The Fuel Fabrication Capability within the U.S. High Performance Research Reactor Conversion Program is funded through the National Nuclear Security Administration (NNSA) NA-26 (Office of Material Management and Minimization). An investigation was commissioned to determine the feasibility of using electroplating techniques to apply a coating of zirconium onto depleted uranium/molybdenum alloy (U-10Mo). Electroplating would provide an alternative method to the existing process of hot roll-bonding zirconium foil onto the U-10Mo fuel foil during the fabrication of fuel elements for high-performance research reactors. The objective of this research was to develop a reproducible and scalable plating process that will produce a uniform, 25 μm thick zirconium metal coating on U-10Mo foil. In previous work, Pacific Northwest National Laboratory (PNNL) established a molten salt electroplating apparatus and protocol to plate zirconium metal onto molybdenum foil (Coffey 2015). During this second year of the research, PNNL furthered this work by moving to the U-10Mo alloy system (90 percent uranium:10 percent molybdenum). The original plating apparatus was disassembled and re-assembled in a laboratory capable of handling low-level radioactive materials. Initially, the work followed the previous year’s approach, and the salt bath composition was targeted at the eutectic composition (LiF:NaF:ZrF4 = 26:37:37 mol%). Early results indicated that the formation of uranium fluoride compounds would be problematic. Other salt bath compositions were investigated in order to eliminate the uranium fluoride production (LiF:NaF = 61:39 mol% and LiF:NaF:KF = 46.5:11.5:42 mol% ). Zirconium metal was used as the crucible for the molten salt. Three plating methods were used—isopotential, galvano static, and pulsed plating. The molten salt method for zirconium metal application provided high-quality plating on molybdenum in PNNL’s previous work. A key advantage of this approach is that

Zirconium elasticity modules

International Nuclear Information System (INIS)

Vavra, G.

1978-01-01

Considered are the limit and the intermediate values of the Young modulus E, modulus of shear G and of linear modulus of compression K obtainable at various temperatures (4.2 to 1133 K) for single crystals of α-zirconium. Determined and presented are the corrected isotropic elasticity characteristics of E, G, K over the above range of temperatures of textured and non-textured α-Zr

Cyclic carbonation calcination studies of limestone and dolomite for CO{sub 2} separation from combustion flue gases - article no. 011801

Energy Technology Data Exchange (ETDEWEB)

Senthoorselvan, S.; Gleis, S.; Hartmut, S.; Yrjas, P.; Hupa, M. [TUM, Garching (Germany)

2009-01-15

Naturally occurring limestone and dolomite samples, originating from different geographical locations, were tested as potential sorbents for carbonation/calcination based CO{sub 2} capture from combustion flue gases. Samples have been studied in a thermogravimetric analyzer under simulated flue gas conditions at three calcination temperatures, viz., 750{sup o}C, 875{sup o}C, and 930{sup o}C for four carbonation calcination reaction (CCR) cycles. The dolomite sample exhibited the highest rate of carbonation than the tested limestones. At the third cycle, its CO{sub 2} capture capacity per kilogram of the sample was nearly equal to that of Gotland, the highest reacting limestone tested. At the fourth cycle it surpassed Gotland, despite the fact that the CaCO{sub 3} content of the Sibbo dolomite was only 2/3 of that of the Gotland. Decay coefficients were calculated by a curve fitting exercise and its value is lowest for the Sibbo dolomite. That means, most probably its capture capacity per kilogram of the sample would remain higher well beyond the fourth cycle. There was a strong correlation between the calcination temperature, the specific surface area of the calcined samples, and the degree of carbonation. It was observed that the higher the calcination temperature, the lower the sorbent reactivity. For a given limestone/dolomite sample, sorbents CO{sub 2} capture capacity depended on the number of CCR cycles and the calcination temperature. According to the equilibrium thermodynamics, the CO{sub 2} partial pressure in the calciner should be lowered to lower the calcination temperature. This can be achieved by additional steam supply into the calciner. Steam could then be condensed in an external condenser to single out the CO{sub 2} stream from the exit gas mixture of the calciner. A calciner design based on this concept is illustrated.

Highly corrosion resistant zirconium based alloy for reactor structural material

International Nuclear Information System (INIS)

Ito, Yoichi.

1996-01-01

The alloy of the present invention is a zirconium based alloy comprising tin (Sn), chromium (Cr), nickel (Ni) and iron (Fe) in zirconium (Zr). The amount of silicon (Si) as an impurity is not more than 60ppm. It is preferred that Sn is from 0.9 to 1.5wt%, that of Cr is from 0.05 to 0.15wt%, and (Fe + Ni) is from 0.17 to 0.5wt%. If not less than 0.12wt% of Fe is added, resistance against nodular corrosion is improved. The upper limit of Fe is preferably 0.40wt% from a view point of uniform suppression for the corrosion. The nodular corrosion can be suppressed by reducing the amount of Si-rich deposition product in the zirconium based alloy. Accordingly, a highly corrosion resistant zirconium based alloy improved for the corrosion resistance of zircaloy-2 and usable for a fuel cladding tube of a BWR type reactor can be obtained. (I.N.)

Method of fabricating zirconium metal for use in composite type fuel cans

International Nuclear Information System (INIS)

Imahashi, Hiromichi; Inagaki, Masatoshi; Akabori, Kimihiko; Tada, Naofumi; Yasuda, Tetsuro.

1985-01-01

Purpose: To mass produce zirconium metal for fuel cans with less radiation hardening. Method: Zirconium sponges as raw material are inserted in a hearth mold and a procedure of melting the zirconium sponges portionwise by using a melting furnace having electron beams as a heat source while moving the hearth is repeated at least for once. Then, the rod-like ingot after melting is melted again in a vacuum or inert gas atmosphere into an ingot of a low oxygen density capable of fabrication. A composite fuel can billet is formed by using the thus obtained zirconium ingot and a zircalloy, and a predetermined composite type fuel can is manufactured by way of hot extrusion and pipe drawing fabrication. The raw material usable herein is zirconium sponge with an oxygen density of 400 ppm or higher and the content of impurity other than oxygen is between 1000 - 5000 ppm in total, or the molten material thereof. (Kamimura, M.)

History of the development of zirconium alloys for use in nuclear reactors

International Nuclear Information System (INIS)

Rickover, H.G.; Geiger, L.D.; Lustman, B.

1975-01-01

The technical problems and the major decisions made during the early development of zirconium alloys for use in naval reactors are outlined. A summary is given of the development of commercial sources of supply for zirconium and hafnium metal over the period 1950 to 1965, and the problems encountered in obtaining zirconium needed for early naval prototype and shipboard reactors are identified. Steps taken in the Government procurement process are described and statistics on production amounts, prices, and inventory are included. Also included are the technical aspects associated with the development of zirconium for water-cooled nuclear reactors, beginning in early 1949 when the Bettis Atomic Power Laboratory was established as a part of the Naval Reactors Program. While in the course of the next 25 years, small-scale investigations were performed on other potential core structural materials such as stainless steel, niobium, aluminum, and beryllium, the pressure for continual development, improvement, and application of zirconium was predominant and unrelenting. (U.S.)

Study of the production of zirconium tetrachloride by chlorination of its oxide

International Nuclear Information System (INIS)

Seo, E.S.M.

1983-01-01

The studies carried out on the production of zirconium tetrachloride by chlorination of pure zirconium oxide with carbon tetrachloride and chlorine in the presence of carbon. In the process of chlorination with carbon tetrachloride, the chlorination efficiency increases with the rise in temperature at intervals between 450 and 750 0 C. The flow of the carbon tetrachloride vapour was 1.50l/min. Higher temperatures of 700 to 850 0 C were used for the zirconium oxide chlorination in the presence of carbon, and the flowrate of the chlorine gas used in the process was 0.50 l/min. Pure zirconium oxide chlorination as well as zirconium oxide - carbon misture chlorination have been studied in connection with the time of reaction at different temperatures and the apparent rate constant, the activation energies, the order of reaction in relation to the concentration of the gases (CCl 4 and Cl 2 ) and the content of carbon in the pellet have all been determined. (Author) [pt

Bioactivity and biocompatibility of hydroxyapatite-based bioceramic coatings on zirconium by plasma electrolytic oxidation

Energy Technology Data Exchange (ETDEWEB)

Aktuğ, Salim Levent, E-mail: saktug@gtu.edu.tr [The Department of Materials Science and Engineering, Gebze Technical University, Gebze, Kocaeli 41400 (Turkey); Durdu, Salih, E-mail: durdusalih@gmail.com [The Department of Industrial Engineering, Giresun University, Merkez, Giresun 28200 (Turkey); Yalçın, Emine, E-mail: emine.yalcin@giresun.edu.tr [The Department of Biology, Giresun University, Merkez, Giresun 28200 (Turkey); Çavuşoğlu, Kültigin, E-mail: kultigin.cavusoglu@giresun.edu.tr [The Department of Biology, Giresun University, Merkez, Giresun 28200 (Turkey); Usta, Metin, E-mail: ustam@gtu.edu.tr [The Department of Materials Science and Engineering, Gebze Technical University, Gebze, Kocaeli 41400 (Turkey); Materials Institute, Marmara Research Center, TUBITAK, Gebze, Kocaeli 41470 (Turkey)

2017-02-01

In the present work, hydroxyapatite (HAP)-based plasma electrolytic oxide (PEO) coatings were produced on zirconium at different current densities in a solution containing calcium acetate and β-calcium glycerophosphate by a single step. The phase structure, surface morphology, functional groups, thickness and roughness of the coatings were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), eddy current method and surface profilometer, respectively. The phases of cubic-zirconia, calcium zirconate and HAP were detected by XRD. The amount of HAP and calcium zirconate increased with increasing current density. The surface of the coatings was very porous and rough. Moreover, bioactivity and biocompatibility of the coatings were analyzed in vitro immersion simulated body fluid (SBF) and MTT (3-(4,5-dimethyl thiazol-2yl)-2,5-diphenyl tetrazolium bromide) assay, hemolysis assay and bacterial formation. The apatite-forming ability of the coatings was evaluated after immersion in SBF up to 28 days. After immersion, the bioactivity of HAP-based coatings on zirconium was greater than the ones of uncoated zirconium and zirconium oxide-based surface. The bioactivity of PEO surface on zirconium was significantly improved under SBF conditions. The bacterial adhesion of the coatings decreased with increasing current density. The bacterial adhesion of the coating produced at 0.370 A/cm{sup 2} was minimum compared to uncoated zirconium coated at 0.260 and 0.292 A/cm{sup 2}. The hemocompatibility of HAP-based surfaces was improved by PEO. The cell attachment and proliferation of the PEO coatings were better than the one of uncoated zirconium according to MTT assay results. - Highlights: • Hydroxyapatite was formed on zirconium at different current densities by single-step plasma electrolytic oxidation. • The amount of hydroxyapatite and calcium-based phases increased with

Stabilized γ-BIMNVOX solid electrolyte: Ethylene glycol–citrate sol–gel synthesis, microwave-assisted calcination, and structural and electrical characterization

Energy Technology Data Exchange (ETDEWEB)

Al-Areqi, Niyazi A.S., E-mail: niyazi.alareqi@gmail.com [Department of Chemistry, Faculty of Applied Science, Taiz University, Taiz, Republic of Yemen (Yemen); Beg, Saba [Department of Chemistry, Aligarh Muslim University, Aligarh 202002 (India); Al-Alas, Ahlam [Department of Chemistry, Faculty of Applied Science, Taiz University, Taiz, Republic of Yemen (Yemen); Hafeez, Shehla [Department of Chemistry, Aligarh Muslim University, Aligarh 202002 (India)

2013-12-25

Highlights: •γ-BIMNVOX was synthesized by ethylene glycol–citrate sol–gel route. •γ-BIMNVOX crystallizes by 25-min microwave-assisted calcination. •Smaller particle sizes for microwave calcined BIMNVOX samples. •Best oxide-ion performance for microwave calcined BIMNVOX samples. -- Abstract: Samples of γ-BIMNVOX (Bi{sub 2}V{sub 1−x}Mn{sub x}O{sub 5.5−x/2}; 0.13 ⩽ x ⩽ 0.20) system were synthesized by an ethylene glycol–citrate sol–gel route. The resulting xerogels were then calcined by the microwave heating using a modified domestic microwave oven operated at 2.45 GHz. Microwave-assisted calcination samples in comparison with other conventionally calcined samples were characterized in terms of phase crystallization, stabilization and particle size using simultaneous thermogravimetric–differential thermal analysis (TG–DTA), X-ray powder diffraction (XRPD) and scanning electron microscopy (SEM). The AC impedance spectroscopy was employed for electrical characterization. It was found that the microwave-assisted calcination route successfully produces better crystalline stabilized γ-BIMNVOX samples with appreciably small average particle sizes after only 25 min of microwave heating. The electrical properties of microwave calcined γ-BIMNVOX system make it an advanced low-temperature solid electrolyte suitable for use in oxide-ion based electrochemical applications.

Decomposition of pre calcined aluminium silicate ores of Afghanistan by hydrochloric acid

International Nuclear Information System (INIS)

Khomidi, A.K.; Mamatov, E.D.

2015-01-01

Present article is devoted to decomposition of pre calcined aluminium silicate ores of Afghanistan by hydrochloric acid. The physicochemical properties of initial aluminium silicate ores were studied by means of X-ray phase, differential thermal and silicate analysis. The chemical composition of aluminium containing ores was determined. The optimal conditions of interaction of initial and pre calcined siallites with hydrochloric acid were defined. The kinetics of acid decomposition of aluminium silicate ores was studied as well.

Development of zirconium alloy tube manufacturing technology

International Nuclear Information System (INIS)

Kim, In Kyu; Park, Chan Hyun; Lee, Seung Hwan; Chung, Sun Kyo

2009-01-01

In late 2004, Korea Nuclear Fuel Company (KNF) launched a government funded joint development program with Westinghouse Electric Co. (WEC) to establish zirconium alloy tube manufacturing technology in Korea. Through this program, KNF and WEC have developed a state of the art facility to manufacture high quality nuclear tubes. KNF performed equipment qualification tests for each manufacturing machine with the support of WEC, and independently carried out product qualification tests for each tube product to be commercially produced. Apart from those tests, characterization test program consisting of specification test and characterization test was developed by KNF and WEC to demonstrate to customers of KNF the quality equivalency of products manufactured by KNF and WEC plants respectively. As part of establishment of performance evaluation technology for zirconium alloy tube in Korea, KNF carried out analyses of materials produced for the characterization test program using the most advanced techniques. Thanks to the accomplishment of the development of zirconium alloy tube manufacturing technology, KNF is expected to acquire positive spin off benefits in terms of technology and economy in the near future

Lithium aluminate/zirconium material useful in the production of tritium

Science.gov (United States)

Cawley, W.E.; Trapp, T.J.

A composition is described useful in the production of tritium in a nuclear reactor. Lithium aluminate particles are dispersed in a matrix of zirconium. Tritium produced by the reactor of neutrons with the lithium are absorbed by the zirconium, thereby decreasing gas pressure within capsules carrying the material.

Design of a hot pilot plant facility for demonstration of the pot calcination process

Energy Technology Data Exchange (ETDEWEB)

Buckham, J A

1962-01-01

A facility was designed for demonstration of the pot calcination process with wastes from processing aluminum alloy fuels, Darex or electrolytic processing of stainless-steel fuels, and Purex processes. This facility will also permit determination of procedures required for economical production of low-porosity, relatively nonleachable materials by addition of suitable reagents to the wastes fed to the calciner. The process consists of concentration by evaporation and thermal decomposition in situ in pots which also serve as the final disposal containers. This unit permits determination of pot loading and density, leachability, melting point, volatile material content, heat release, and thermal conductivity of the calcine. Also to be determined are transient calcine temperature distributions, fission product behavior during calcination, deentrainment obtained in the various parts of the system, decontamination achieved on all liquid and gaseous effluent streams, need for venting of stored pots, optimum means of remotely sealing the pots, and methods required for production of a minimum volume of noncondensable off-gas. This facility will employ nominal full-scale pots 8 and 12 in. in diameter and 8 ft long. A unique evaporator design was evolved to permit operation either with close-coupled continuous feed preparation or with bath feed preparation. Provisions were made to circumvent possible explosions due to organic material in feed solutions and other suspected hazards.

Anticorrosive Behavior and Porosity of Tricationic Phosphate and Zirconium Conversion Coating on Galvanized Steel

Science.gov (United States)

Velasquez, Camilo S.; Pimenta, Egnalda P. S.; Lins, Vanessa F. C.

2018-05-01

This work evaluates the corrosion resistance of galvanized steel treated with tricationic phosphate and zirconium conversion coating after painting, by using electrochemical techniques, accelerated and field corrosion tests. A non-uniform and heterogeneous distribution of zirconium on the steel surface was observed due to preferential nucleation of the zirconium on the aluminum-rich sites on the surface of galvanized steel. The long-term anti-corrosion performance in a saline solution was better for the phosphate coating up to 120 days. The coating capacitance registered a higher increase for the zirconium coatings than the phosphate coatings up to 120 days of immersion. This result agrees with the higher porosity of zirconium coating in relation to the phosphate coating. After 3840 h of accelerated corrosion test, and after 1 year of accelerated field test, zirconium-treated samples showed an average scribe delamination length higher than the phosphate-treated samples.

Thermodynamic Database for Zirconium Alloys

International Nuclear Information System (INIS)

Jerlerud Perez, Rosa

2003-05-01

For many decades zirconium alloys have been commonly used in the nuclear power industry as fuel cladding material. Besides their good corrosion resistance and acceptable mechanical properties the main reason of using these alloys is the low neutron absorption. Zirconium alloys are exposed to a very severe environment during the nuclear fission process and there is a demand for better design of this material. To meet this requirement a thermodynamic database is developed to support material designers. In this thesis some aspects about the development of a thermodynamic database for zirconium alloys are presented. A thermodynamic database represents an important facility in applying thermodynamic equilibrium calculations for a given material providing: 1) relevant information about the thermodynamic properties of the alloys e.g. enthalpies, activities, heat capacity, and 2) significant information for the manufacturing process e.g. heat treatment temperature. The basic information in the database is first the unary data, i.e. pure elements; those are taken from the compilation of the Scientific Group Thermodata Europe (SGTE) and then the binary and ternary systems. All phases present in those binary and ternary systems are described by means of the Gibbs energy dependence on composition and temperature. Many of those binary systems have been taken from published or unpublished works and others have been assessed in the present work. All the calculations have been made using Thermo C alc software and the representation of the Gibbs energy obtained by applying Calphad technique

Processing of concentrated radioactive wastes into cement and bitumens following calcination

International Nuclear Information System (INIS)

Napravnik, J.; Sazavsky, P.; Ditl, P.; Prikryl, P.

1985-01-01

A brief characteristic is presented of the most frequently used processes of solidification of liquid radioactive wastes, viz., bituminization, cementation and their combination with calcination. The effect of individual parameters is assessed on the choice of the type of solidification process as is their importance in the actual process, in temporary storage, during transportation and under conditions of long-term storage. It has been found that a combination of the procedures could lead to a modular system of methods and equipment. This would allow to approach optimal solidification of wastes in the present period and to establish a research reserve for the development of more modern, economically advantageous and safer procedures. A rough estimate is made of the costs of the solidification of 1 m 3 of radioactive concentrate from the V-1 power plant at a production of 380 m 3 /year, this for the cementation-calcination and bituminization-calcination procedures. The said rough economic analysis only serves to identify the major operating components which have the greatest effect on the economic evaluation of the solidification procedures. (Z.M.)

Calcined clay lightweight ceramics made with wood sawdust and sodium silicate

Energy Technology Data Exchange (ETDEWEB)

Santis, Bruno Carlos de; Rossignolo, Joao Adriano, E-mail: desantis.bruno@gmail.com [Universidade de Sao Paulo (USP), Pirassununga, SP (Brazil); Morelli, Marcio Raymundo [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Departamento de Engenharia de Materiais

2016-11-15

This paper aims to study the influence of including wood sawdust and sodium silicate in the production process of calcined clay lightweight ceramics. In the production process first, a sample used by a company that produces ceramic products in Brazil was collected. The sample was analysed by techniques of liquidity (LL) and plasticity (LP) limits, particle size analysis, specific mass, X-ray diffraction (XRD) and X ray fluorescence spectrometry (XRF). From the clay, specimens of pure clay and mixtures with wood sawdust (10%, 20% and 30% by mass) and sodium silicate were produced and fired at a temperature of 900 deg C. These specimens were submitted to tests of water absorption, porosity, specific mass and compressive strength. Results of this research indicate that the incorporation of wood sawdust and sodium silicate in the ceramic paste specimens can be useful to make calcined clay lightweight ceramics with special characteristics (low values of water absorption and specific mass and high values of compressive strength), which could be used to produce calcined clay lightweight aggregates to be used in structural concrete. (author)

low dose irradiation growth in zirconium

International Nuclear Information System (INIS)

Fortis, A.M.

1987-01-01

Low dose neutron irradiation growth in textured and recrystallized zirconium, is studied, at the Candu Reactors Calandria temperature (340 K) and at 77 K. It was necessary to design and build 1: A facility to irradiate at high temperatures, which was installed in the Argentine Atomic Energy Commission's RA1 Reactor; 2: Devices to carry out thermal recoveries, and 3: Devices for 'in situ' measurements of dimensional changes. The first growth kinetics curves were obtained at 365 K and at 77 K in a cryostat under neutron fluxes of similar spectra. Irradiation growth experiments were made in zirconium doped with fissionable material (0,1 at % 235 U). In this way an equivalent dose two orders of magnitude greater than the reactor's fast neutrons dose was obtained, significantly reducing the irradiation time. The specimens used were bimetallic couples, thus obtaining a great accuracy in the measurements. The results allow to determine that the dislocation loops are the main cause of irradiation growth in recrystallized zirconium. Furthermore, it is shown the importance of 'in situ' measurements as a way to avoid the effect that temperature changes have in the final growth measurement; since they can modify the residual stresses and the overconcentrations of defects. (M.E.L.) [es

Study of zirconium-addition binary systems

International Nuclear Information System (INIS)

Wozniakova, B.; Kuchar, L.

1975-01-01

The curves are given of the solid and the liquid of binary zirconium-addition systems. Most additions reduce the melting temperature of zirconium. The only known additions to increase the melting temperature are nitrogen, oxygen and hafnium. Also given are the transformation curves of the systems and the elements are given which reduce or raise the temperature of α-β transformation. From the Mendeleev table into which are plotted the curves of the solid and the liquid of binary systems it is possible to predict the properties of unknown binary systems. For the calculations of the curves of the solid and the liquid, 1860 degC was taken as the temperature of zirconium melting. For the calculations of transformation curves, 865 degC was taken as the temperature of α-β transformation. The equations are given of the curves of the solid and the liquid and of the transformation curves of some Zr-addition systems. Also given are the calculated equilibrium distribution coefficients and the equilibrium distribution coefficients of the transformation of additions in Zr and their limit values for temperatures approximating the melting point or the temperature of the transformation of pure Zr, and the values pertaining to eutectic and peritectic or eutectoid and peritectoid temperatures. (J.B.)

Bioremediation of zirconium from aqueous solution by coriolus versicolor: process optimization

International Nuclear Information System (INIS)

Amin, M.; Bhatti, H. N.; Sadaf, S.

2013-01-01

In the present study the potential of live mycelia of Coriolus versicolor was explored for the removal of zirconium from simulated aqueous solution. Optimum experimental parameters for the bioremediation of zirconium using C. versicolor biomass have been investigated by studying the effect of mycelia dose, concentration of zirconium, contact time and temperature. The isothermal studies indicated that the ongoing bioremediation process was exothermic in nature and obeyed Langmuir adsorption isotherm model. The Gibbs free energy (ΔG), entropy (ΔS) and enthalpy (ΔH) of bioremediation were also determined. The result showed that bioremediation of zirconium by live C. versicolor was feasible and spontaneous at room temperature. The equilibrium data verified the involvement of chemisorption during the bioremediation. The kinetic data indicated the operation of pseudo-second order process during the biosorption of zirconium from aqueous solution. Maximum bioremediation capacity (110.75 mg/g) of C. versicolor was observed under optimum operational conditions: pH 4.5, biomass dose 0.05 mg/100 mL, contact time 6 h and temperature 30 degree C. The results showed that C. versicolor could be used for bioremediation of heavy metal ions from aqueous systems. (author)

Evaluation of a Zirconium Recycle Scrubber System

Energy Technology Data Exchange (ETDEWEB)

Spencer, Barry B. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Bruffey, Stephanie H. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2017-04-01

A hot-cell demonstration of the zirconium recycle process is planned as part of the Materials Recovery and Waste Forms Development (MRWFD) campaign. The process treats Zircaloy® cladding recovered from used nuclear fuel with chlorine gas to recover the zirconium as volatile ZrCl4. This releases radioactive tritium trapped in the alloy, converting it to volatile tritium chloride (TCl). To meet regulatory requirements governing radioactive emissions from nuclear fuel treatment operations, the capture and retention of a portion of this TCl may be required prior to discharge of the off-gas stream to the environment. In addition to demonstrating tritium removal from a synthetic zirconium recycle off-gas stream, the recovery and quantification of tritium may refine estimates of the amount of tritium present in the Zircaloy cladding of used nuclear fuel. To support these objectives, a bubbler-type scrubber was fabricated to remove the TCl from the zirconium recycle off-gas stream. The scrubber was fabricated from glass and polymer components that are resistant to chlorine and hydrochloric acid solutions. Because of concerns that the scrubber efficiency is not quantitative, tests were performed using DCl as a stand-in to experimentally measure the scrubbing efficiency of this unit. Scrubbing efficiency was ~108% ± 3% with water as the scrubber solution. Variations were noted when 1 M NaOH scrub solution was used, values ranged from 64% to 130%. The reason for the variations is not known. It is recommended that the equipment be operated with water as the scrubbing solution. Scrubbing efficiency is estimated at 100%.

Study on the scattering law and scattering kernel of hydrogen in zirconium hydride

International Nuclear Information System (INIS)

Jiang Xinbiao; Chen Wei; Chen Da; Yin Banghua; Xie Zhongsheng

1999-01-01

The nuclear analytical model of calculating scattering law and scattering kernel for the uranium zirconium hybrid reactor is described. In the light of the acoustic and optic model of zirconium hydride, its frequency distribution function f(ω) is given and the scattering law of hydrogen in zirconium hydride is obtained by GASKET. The scattering kernel σ l (E 0 →E) of hydrogen bound in zirconium hydride is provided by the SMP code in the standard WIMS cross section library. Along with this library, WIMS is used to calculate the thermal neutron energy spectrum of fuel cell. The results are satisfied

Preparation and Characterization of Hydrous Zirconium Oxide Formed by Homogeneous Precipitation

Directory of Open Access Journals (Sweden)

Silva G.L.J.P. da

2002-01-01

Full Text Available This paper reports on the preparation, characterization and study of the ion exchange behavior of hydrous zirconium oxides formed by homogeneous precipitation from zirconium oxychloride. The precipitants used were obtained by thermal decomposition of urea, sodium nitrite or ammonium carbonate. Seven compounds were prepared and characterized by thermal analysis, X-ray diffractometry and by surface area measurements. Amorphous forms were obtained in each case, a result that agrees with those obtained by conventional gel precipitation methodology. All these materials present surface area values of >148 m².g-1, determined after heat treatment at 50 °C. The ion exchange behavior of each hydrous zirconium oxide prepared was studied using K+ as the exchanged species and the results compared with those obtained for hydrous zirconium oxide originally precipitated by the sol gel method.

Calcinated tea and cellulose composite films and its dielectric and lead adsorption properties.

Science.gov (United States)

Jayaramudu, Tippabattini; Varaprasad, Kokkarachedu; Kim, Hyun Chan; Kafy, Abdullahil; Kim, Jung Woong; Kim, Jaehwan

2017-09-01

In this paper, calcinated tea and cellulose composite (CTCC) films were fabricated via solution casting method. Chemical structure, morphology, crystallinity and thermal stability of the fabricated films were characterized by using Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and thermogravimetric analysis. The effect of calcinated tea loading on the properties of the prepared CTCC films was studied. The results suggest that the prepared CTCC films show higher mechanical properties, thermal stability and dielectric constant than the neat cellulose film. In addition, the CTCC films adsorb Pb 2+ ions and its adsorption performance depends on the calcinated tea content and pH level. The CTCC films are useful for sensors, flexible capacitor as well as lead adsorption applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Methods of studying oxide scales grown on zirconium alloys in autoclaves and in a PWR

International Nuclear Information System (INIS)

Blank, H.; Bart, G.; Thiele, H.

1992-01-01

The analysis of water-side corrosion of zirconium alloys has been a field of research for more than 25 years, but the details of the mechanisms involved still cannot be put into a coherent picture. Improved methods are required to establish the details of the microstructure of the oxide scales. A new approach has been made for a general analysis of oxide specimens from scales grown on the zirconium-based cladding alloys of PWR rods in order to analyse the morphology of these scales, the topography of the oxide/metal interface and the crystal structures close to this interface: a) Instead of using the conventional pickling solutions, the Zr-alloys are dissolved using a 'softer' solution (Br 2 in an organic solvent) in order to avoid damage to the oxide at the oxide/metal interface to be analysed by SEM (scanning electron microscopy). A second advantage of this method is easy etching of the grain structure of Zr-alloys for SEM analysis; b) By using the particular properties of the oxide scales, the corrosion-rate-determining innermost part of the oxide layer at the oxide/metal interface can be separated from the rest of the oxide scale and then analysed by SEM, STEM (scanning transmission electron microscopy), TEM (transmission electron microscopy) and electron diffraction after dissolution of the alloy. Examples are given from oxides grown on Zr-alloys in a pressurized water reactor and in autoclaves. (author) 8 figs., 3 tabs., 9 refs

Synthesis, characterization and optical properties of novel N donor ligands-chelated zirconium(IV) complexes

Science.gov (United States)

Shahroosvand, Hashem; Nasouti, Fahimeh; Mohajerani, Ezeddin; Khabbazi, Amir

2012-11-01

Novel zirconium complexes have been synthesized by using a mixture of zirconium nitrate, 1,2,4,5-benzen tetracarboxylic acid (H4btec), 1,10-phenanthroline(phen) and potassium thiocyanate. Monodentate coordination mode of btec acid for all complexes was investigated by FT-IR spectroscopy. The complexes were also characterized by UV-Vis, 1H NMR, CHN, ICP-AES. The reaction details and features were described and discussed. The photoluminescence emission of seven zirconium complexes was shown two series peaks: first, sharp and intense bands from 300 to 500 nm and broadened with less intensity from 650 to 750 nm for the second bands. Each of the zirconium compounds were doped in PVK:PBD blend as host. The ratio of zirconium complexes for each type were modified 8 wt.% in PVK:PBD(100:40). The electroluminescence spectra of zirconium complexes were indicated a red shift rather than PVK:PBD blend. We suggest that the electroplex occurring at PVK-Zr complex interface.

The variation of cationic microstructure in Mn-doped spinel ferrite during calcination and its effect on formaldehyde catalytic oxidation

Energy Technology Data Exchange (ETDEWEB)

Liang, Xiaoliang [CAS Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Guangdong Provincial Key Laboratory of Mineral Physics and Materials, Guangzhou 510640 (China); Liu, Peng [CAS Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Guangdong Provincial Key Laboratory of Mineral Physics and Materials, Guangzhou 510640 (China); He, Hongping, E-mail: hehp@gig.ac.cn [CAS Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Guangdong Provincial Key Laboratory of Mineral Physics and Materials, Guangzhou 510640 (China); Wei, Gaoling [Guangdong Institute of Eco-Environmental and Soil Sciences, Guangzhou 510650 (China); Chen, Tianhu [School of Resources and Environmental Engineering, Hefei University of Technology, Hefei 230009 (China); Tan, Wei; Tan, Fuding [CAS Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Guangdong Provincial Key Laboratory of Mineral Physics and Materials, Guangzhou 510640 (China); Zhu, Jianxi; Zhu, Runliang [CAS Key Laboratory of Mineralogy and Metallogeny, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Guangdong Provincial Key Laboratory of Mineral Physics and Materials, Guangzhou 510640 (China)

2016-04-05

Highlights: • Calcination causes the activity variation of Mn-doped ferrites for HCHO oxidation. • The variation of catalytic activity of ferrites by calcination is non-linear. • Mn enriches on the calcinated ferrite surface in the valence of +3 and +4. • The reduction temperature of surface Mn{sup 4+} species is well correlated to T50. - Abstract: In this study, a series of Mn substituted spinel ferrites calcinated at different temperatures were used as catalysts for the oxidation of formaldehyde (HCHO). X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy and H{sub 2} temperature-programmed reduction were conducted to characterize the structure and physico-chemical properties of catalysts, which were affected by calcination in the range of 200–600 °C. Results show that all the ferrites were with spinel structure, and those calcinated in the range of 300–600 °C were in the phase of maghemite. The calcination changed the valence and distribution of Mn and Fe on the ferrite surface, and accordingly the reducibility of ferrites. The HCHO catalytic oxidation test showed that with the increase of calcination temperature, the activity was initially improved until 400 °C, but then decreased. The variation of HCHO conversion performance was well positively correlated to the variation of reduction temperature of surface Mn{sup 4+} species. The remarkable effect of calcination on the catalytic activity of Mn-doped spinel ferrites for HCHO oxidation was discussed in view of reaction mechanism and variations in cationic microstructure of Mn-doped ferrites.

The variation of cationic microstructure in Mn-doped spinel ferrite during calcination and its effect on formaldehyde catalytic oxidation

International Nuclear Information System (INIS)

Liang, Xiaoliang; Liu, Peng; He, Hongping; Wei, Gaoling; Chen, Tianhu; Tan, Wei; Tan, Fuding; Zhu, Jianxi; Zhu, Runliang

2016-01-01

Highlights: • Calcination causes the activity variation of Mn-doped ferrites for HCHO oxidation. • The variation of catalytic activity of ferrites by calcination is non-linear. • Mn enriches on the calcinated ferrite surface in the valence of +3 and +4. • The reduction temperature of surface Mn"4"+ species is well correlated to T50. - Abstract: In this study, a series of Mn substituted spinel ferrites calcinated at different temperatures were used as catalysts for the oxidation of formaldehyde (HCHO). X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy and H_2 temperature-programmed reduction were conducted to characterize the structure and physico-chemical properties of catalysts, which were affected by calcination in the range of 200–600 °C. Results show that all the ferrites were with spinel structure, and those calcinated in the range of 300–600 °C were in the phase of maghemite. The calcination changed the valence and distribution of Mn and Fe on the ferrite surface, and accordingly the reducibility of ferrites. The HCHO catalytic oxidation test showed that with the increase of calcination temperature, the activity was initially improved until 400 °C, but then decreased. The variation of HCHO conversion performance was well positively correlated to the variation of reduction temperature of surface Mn"4"+ species. The remarkable effect of calcination on the catalytic activity of Mn-doped spinel ferrites for HCHO oxidation was discussed in view of reaction mechanism and variations in cationic microstructure of Mn-doped ferrites.

An evaluated neutronic data file for elemental zirconium

International Nuclear Information System (INIS)

Smith, A.B.; Chiba, S.

1994-09-01

A comprehensive evaluated neutronic data file for elemental zirconium is derived and presented in the ENDF/B-VI formats. The derivation is based upon measured microscopic nuclear data, augmented by model calculations as necessary. The primary objective is a quality contemporary file suitable for fission-reactor development extending from conventional thermal to fast and innovative systems. This new file is a significant improvement over previously available evaluated zirconium files, in part, as a consequence of extensive new experimental measurements reported elsewhere

Effect of zirconium addition on the recrystallization behaviour of a ...

Indian Academy of Sciences (India)

In the present work, zirconium was added to a commercial Al–Cu–Mg alloy and by heat treatment Al3Zr particles were precipitated and after forging, the grain size was an order of magnitude lower than the alloy without zirconium. Transmission electron microscopy was employed to characterize the second phase particles, ...

Ce - promoted catalyst from hydrotalcites for CO2 reforming of methane: calcination temperature effect

Directory of Open Access Journals (Sweden)

Carlos Enrique Daza

2012-01-01

Full Text Available Ce-promoted Ni-catalysts from hydrotalcites were obtained. The effect of calcination temperature on the chemical and physical properties of the catalysts was studied. Several techniques were used to determine the chemical and physical characteristics of oxides. The apparent activation energies of reduction were determined. Catalytic experiments at 48 L g-1h-1 without pre-reduction in CO2 reforming of methane were performed. The spinel-like phase in these oxides was only formed at 1000 ºC. The reduction of Ni2+ in the oxides was clearly affected by the calcination temperature which was correlated with catalytic performance. The catalyst calcined at 700 ºC showed the greatest activity.

Calcined eggshell (CES): An efficient natural catalyst for ...

Indian Academy of Sciences (India)

hydes with active methylene compounds using calcined eggshell (CES) as an efficient ... of the important reactions to achieve carbon–carbon ... solid catalyst for biodiesel production,24 as a catalyst ... which supports for adsorption of water on CaO and ... The organic phase .... After extraction of the product with ethylac-.

Microwave energy for post-calcination treatment of high-level nuclear wastes

International Nuclear Information System (INIS)

Gombert, D.; Priebe, S.J.; Berreth, J.R.

1980-01-01

High-level radioactive wastes generated from nuclear fuel reprocessing require treatment for effective long-term storage. Heating by microwave energy is explored in processing of two possible waste forms: (1) drying of a pelleted form of calcined waste; and (2) vitrification of calcined waste. It is shown that residence times for these processes can be greatly reduced when using microwave energy rather than conventional heating sources, without affecting product properties. Compounds in the waste and in the glass frit additives couple very well with the 2.45 GHz microwave field so that no special microwave absorbers are necessary

Volatilization and trapping of ruthenium during calcination of nitric acid solutions

International Nuclear Information System (INIS)

Klein, M.; Weyers, C.; Goossens, W.R.A.; Smet, M. de; Trine, J.

1983-01-01

Solid radioactive aerosols and semi-volatile fission products e.g. Ru, Cs, Sb are generated during high level liquid waste calcination and vitrification processes. The retention of Ruthenium was studied because of its strong tendency to form volatile compounds in oxidative media. Since RuO 4 was the suspected form for high temperature processes, the study was carried out on the behaviour of RuO 4 and its retention on adsorbants and catalysts for various gas compositions. The behaviour of volatilized Ru species obtained by calcination of nitrosyl Ru compounds was then compared with the RuO 4 case

Fuzzy modeling and control of the calcination process in a kiln

International Nuclear Information System (INIS)

Ramirez, M.; Haber, R.

1999-01-01

Calcination kilns are strongly nonlinear, multivariable processes, that only can be modeled with great uncertainty. In order to get a quality product and ensure the process efficiency, the controller must keep a prescribed temperature profile optimizing the fuel consumption. In this paper, a design methodology of a multivariable fuzzy controller for a nickel calcination kiln is presented. The controller structure is a classical one, and uses the Mamdani fuzzy inference system. In simulation results the fuzzy controller exhibits a great robustness in presence of several types of disturbances, and a better performance than the PID in same conditions is observed. (author)

The addition zirconium effect on the solubility and activity of sulfur in liquid iron

International Nuclear Information System (INIS)

Burylev, B.P.; Mojsov, L.P.

1994-01-01

Critical analysis of reference data on thermodynamic properties of zirconium sulfides is conducted for evaluation of zirconium desulfonation ability in liquid steel. Sulfur solubility dependence on zirconium concentration in liquid iron is presented. Curves of sulfur solubility in liquid iron in the presence of other elements, including titanium, manganese, vanadium and chromium are presented for comparison. It is shown that equilibrium concentration of sulfur is much lower than standard sulfur concentrations in steel, therefore zirconium appears to be the best desulfonator among the metals considered

A microstuctural study on accelerated zirconium alloy oxidation

International Nuclear Information System (INIS)

Sohn, Seung Bum; Oh, Seung Jun; Jang, Jung Nam; Kim, Yong Soo; Jung, Yong Hwan; Baek, Jong Hyuk; Park, Jung Yong

2005-01-01

It has been reported that the effect of thermal redistribution of hydrides across the zirconium metaloxide interface, coupled with thermal feedback on the metal-oxide interface, is a dominating factor in the accelerated oxidation in zirconium alloys cladding PWR fuel. Basically this influence determines characteristic of oxide layer. Influence estimation for corrosion oxide layer due to hydrogen / hydride carried out because of investigation on the kinetic on accelerated oxidation due to hydride precipitation was preceded. Generally, it is known that ZrO 2 tetragonal layer structures play an important role as a barrier layer. So analysing the ZrO 2 monoclinic and tetragonal structure distribution is our main aim. Especially, this study focused on the hydride effects. In other words, the difference of crystal structure distribution between pre-hydrided and without hydrided specimen is just expected results. Experimental results of microstructure at zirconium metal-oxide interface through TEM and EBSD analysis was confirmed

Development of tantalum–zirconium alloy for hydrogen purification

Energy Technology Data Exchange (ETDEWEB)

Kumar, Sanjay, E-mail: sanjay.barc@gmail.com [Fusion Reactor Materials Section, MG, BARC, Mumbai 85 (India); IAMR, Hiroshima University, Higashihiroshima 739-8530 (Japan); Singh, Anamika [GSASM Hiroshima University, Higashihiroshima 739-8530 (Japan); Jain, Uttam; Dey, Gautam Kumar [Fusion Reactor Materials Section, MG, BARC, Mumbai 85 (India)

2016-11-01

Highlights: • Terminal solid solubility of Ta increases with Zr addition. • Increase in lattice parameters of Ta due to Zr addition may be the possible reason. • Enhance H solubility could also be explained on the change in e-DOS of Ta–Zr alloys. • Ta–Zr alloys could be possible combination for hydrogen purification membrane. - Abstract: Terminal solid solubility of hydrogen in Ta–Zr alloys has been studied in connection with the development of tantalum based metallic membrane for hydrogen/tritium purification. The alloys were prepared by vacuum arc melting technique and subsequently cold rolled to 0.2 mm thickness. The terminal solid solubility of hydrogen in these cold rolled samples was investigated in a modified Sieverts apparatus. The terminal solid solubility of hydrogen was marginally increased with zirconium content. The change in the lattices parameter of tantalum upon zirconium addition and the higher affinity of zirconium for hydrogen as compared to tantalum could be the possible reasons.

Zirconium determination in refractories (gravimetric method)

International Nuclear Information System (INIS)

Capiotto, N.; Narahashi, Y.; Perish, P.G.; Souza, J.R. de

1991-01-01

A gravimetric method for zirconium determination in refractories is described. X-ray fluorescence analysis is also employed in this experiment and considerations about interfering elements are presented. (M.V.M.)

Study of the production of Zirconium tetracheoride by chlorination of its oxide

International Nuclear Information System (INIS)

Seo, E.S.M.; Abrao, A.

1987-08-01

This work describes the studies carried out on the production of zirconium tetrachloride by chlorianation of pure zirconium oxide with (a) carbon tetrachloride and (b) chlorine in the presence of carbon. In the process of chlorination with carbon tetrachloride it has been determined that efficiency increases with the rising of temperature between 450 and 750 0 C. The flow rate of the carbon tetrachloride vapour used was 1.50L/min. For the zirconium oxide chlorination in the presence of carbon, the study has been carried out at temperatures between 700 and 850 0 C and the flow rate of the chlorine gas used in the process was 0,50/Lmin. Pure zirconium oxide chlorination as well as zirconium oxide-carbon mixture chlrorination have been studied in connection with the time of reaction at different temperatures and the apparent rate constants, the activation energies, the order of reaction in relation to the concentration of the gases (CCl 4 and Cl 2 ) and the content of carbon in the pellet have all been determined. (Author) [pt

Role of Calcination Temperature on the Hydrotalcite Derived MgO–Al2O3 in Converting Ethanol to Butanol

Energy Technology Data Exchange (ETDEWEB)

Ramasamy, Karthikeyan K.; Gray, Michel J.; Job, Heather M.; Santosa, Daniel M.; Li, Xiaohong S.; Devaraj, Arun; Karkamkar, Abhijeet J.; Wang, Yong

2015-10-09

In the base catalyzed ethanol condensation reactions, the calcined MgO-Al₂O₃ derived hydrotalcites used broadly as catalytic material and the calcination temperature plays a big role in determining the catalytic activity. The characteristic of the hydrotalcite material treated between catalytically relevant temperatures 450ºC and 800ºC have been studied with respect to the physical, chemical, and structural properties and compared with catalytic activity testing. With the increasing calcination temperature, the total measured catalytic basicity dropped linearly with the calcination temperature and the total measured acidity stayed the same for all the calcination temperatures except 800ºC. However, the catalyst activity testing does not show any direct correlation between the measured catalytic basicity and the catalyst activity to the ethanol condensation reaction to form 1-butanol. The highest ethanol conversion of 44 percent with 1-butanol selectivity of 50 percent was achieved for the 600ºC calcined hydrotalcite material.

Synthesis of alumina powder with seeds by Pechini Method using O2 as calcination atmosphere

International Nuclear Information System (INIS)

Salem, R.E.P.; Guilherme, K.A.; Chinelatto, A.S.A.; Chinelatto, A. L.

2012-01-01

Alumina is a very investigated material due to its excellent refractory characteristics and mechanical properties. Its alpha phase, the most stable one, has a formation temperature of about 1200 ° C. Due to its high temperature of formation, many researches have been trying to reduce it through addition of seeds of alpha phase in chemical processes of synthesis. This work aims to synthesize ultrafine powders of alpha-alumina by the Pechini method with seeding, and using an O 2 atmosphere in the pre-calcination (500 ° C) and calcination (1000 ° C and 1100° C) steps. The resulting powders were characterized through X-ray diffractometry, infrared spectroscopy and scanning electron microscopy. The results were compared with samples calcined on ai. It was verified that the presence of oxygen in the calcination atmosphere favored the elimination of residual carbon from the precursor powders, forthcoming from the great amount of organic material used on the synthesis, modifying its morphology and favoring reduction of particle size. (author)

Fluorimetric determination of uranium in zirconium and zircaloy alloys

International Nuclear Information System (INIS)

Acosta L, E.

1991-05-01

The objective of this procedure is to determine microquantities of uranium in zirconium and zircaloy alloys. The report also covers the determination of uranium in zirconium alloys and zircaloy in the range from 0.25 to 20 ppm on 1 g of base sample of radioactive material. These limit its can be variable if the size of the used aliquot one is changed for the final determination of uranium. (Author)

Alkylation of isobutane by butenes on zirconium sulfate catalysts

International Nuclear Information System (INIS)

Lavrenov, A.V.; Perelevskij, E.V.; Finevich, V.P.; Zajkovskij, V.I.; Paukshtis, E.A.; Duplyakiv, V.K.; Bal'zhinimaev, B.S.

2003-01-01

Preparation of applied zirconium sulfate catalysts obtained by the method of impregnation is investigated. Results of comparative study of structural, acid-base and catalytic properties of sulfated zirconium dioxide applied on silica gel and aluminium oxide are represented. Intervals of values of synthesis basic parameters and characteristics of catalysts properties providing achievement of high activity and selectivity in isobutane alkylation by butenes in liquid phase are determined [ru

Preparation of zirconium molybdate gel generator

International Nuclear Information System (INIS)

Charoen, S.; Aungurarat, G.; Laohawilai, S.; Sukontpradit, W.; Jingjit, S.

1994-01-01

A procedure for preparation of 99mTc generator based on conversion to zirconium molybdate gel of 99Mo produced by neutron activation was reported. The gel was prepared from zirconium oxychloride solution pH 1.6, ammonium molybdate solution pH 3-5 and mole ratio of Zr:Mo 1:1 which had water content about 7-8%. Small generators containing 1-1.5 g of gel were eluted with average efficiencies of 77% and the activity peak in the first 3 ml of 10 ml of saline solution. The amount of Mo and Zr in eluates were below the acceptance limit. The gel generators of activity about 100 mCi were prepared and had the good performance in elutability and stability

Sorption of Europium in zirconium silicate

International Nuclear Information System (INIS)

Garcia R, G.

2004-01-01

Some minerals have the property of sipping radioactive metals in solution, that it takes advantage to manufacture contention barriers that are placed in the repositories of nuclear wastes. The more recent investigations are focused in the development of new technologies guided to the sorption of alpha emissors on minerals which avoid their dispersion in the environment. In an effort to contribute to the understanding of this type of properties, some studies of sorption of Europium III are presented like homologous of the americium, on the surface of zirconium silicate (ZrSiO 4 ). In this work the results of sorption experiences are presented as well as the interpretation of the phenomena of the formation of species in the surface of the zirconium silicate. (Author)

ICPP radioactive liquid and calcine waste technologies evaluation final report and recommendation

Energy Technology Data Exchange (ETDEWEB)

NONE

1995-04-01

Using a formalized Systems Engineering approach, the Latched Idaho Technologies Company developed and evaluated numerous alternatives for treating, immobilizing, and disposing of radioactive liquid and calcine wastes at the Idaho Chemical Processing Plant. Based on technical analysis data as of March, 1995, it is recommended that the Department of Energy consider a phased processing approach -- utilizing Radionuclide Partitioning for radioactive liquid and calcine waste treatment, FUETAP Grout for low-activity waste immobilization, and Glass (Vitrification) for high-activity waste immobilization -- as the preferred treatment and immobilization alternative.

Study of as-synthesized and calcined hydrocalumites as possible ...

Indian Academy of Sciences (India)

Administrator

ments. Finally, these solids were tested as antacids by using a synthetic gastric juice. Results showed that calcined samples were able to neutralize the synthetic gastric juice in more extension as an as-synthesized ..... D 2010 Appl. Clay Sci.

Films of double oxides of zirconium and iron

International Nuclear Information System (INIS)

Kozik, V.V.; Borilo, L.P.; Shul'pekov, A.M.

2000-01-01

Films of double oxides of zirconium and iron were prepared by the method of precipitation from film-forming alcohol solutions of zirconium oxychloride and iron chloride with subsequent thermal treatment. Using the methods of X-ray phase and differential thermal analyses, conductometry and optical spectroscopy, basic chemical processes occurring in the film-forming solutions and during thermal treatment are studied alongside with phase composition and optical characteristics of the films prepared. The composition-property diagrams of the given system in a thin-film state are plotted [ru

Determination of the Rate of Formation of Hydroceramic Waste Forms made with INEEL Calcined Wastes; FINAL

International Nuclear Information System (INIS)

Barry Scheetz; Johnson Olanrewaju

2001-01-01

The formulation, synthesis, characterization and hydration kinetics of hydroceramic waste forms designed as potential hosts for existing INEEL calcine high-level wastes have been established as functions of temperature and processing time. Initial experimentations were conducted with several aluminosilicate pozzolanic materials, ranging from fly ash obtained from various power generating coal and other combustion industries to reactive alumina, natural clays and ground bottled glass powders. The final selection criteria were based on the ease of processing, excellent physical properties and chemical durability (low-leaching) determined from the PCT test produced in hydroceramic. The formulation contains vermiculite, Sr(NO32), CsC1, NaOH, thermally altered (calcined natural clay) and INEEL simulated calcine high-level nuclear wastes and 30 weight percent of fluorinel blend calcine and zirconia calcine. Syntheses were carried out at 75-200 degree C at autogeneous water pressure (100% relative humidity) at various time intervals. The resulting monolithic compact products were hard and resisted breaking when dropped from a 5 ft height. Hydroceramic host mixed with fluorinel blend calcine and processed at 75 degree C crumbled into rice hull-side grains or developed scaly flakes. However, the samples equally possessed the same chemical durability as their unbroken counterparts. Phase identification by XRD revealed that hydroceramic host crystallized type zeolite at 75-150 degree C and NaP1 at 175-200 degree C in addition to the presence of quartz phase originating from the clay reactant. Hydroceramic host mixed with either fluorinel blend calcine or zirconia calcine crystallized type A zeolite at 75-95 degree C, formed a mixture of type A zeolite and hydroxysodalite at 125-150 degree C and hydroxysodalite at 175-200 degree C. Quartz, calcium fluoride and zirconia phases from the clay reactant and the two calcine wastes were also detected. The PCT test solution

Radiochemical determination of zirconium by inductively coupled plasma mass spectrometry (ICPMS)

International Nuclear Information System (INIS)

Oliveira, Thiago C.; Oliveira, Arno Heeren de

2013-01-01

The zirconium isotope 93 Zr is a long-lived pure β-particle-emitting radionuclide thus occurring as one of the radionuclides found in nuclear reactors. It's produced from 235 U fission and from 92 Zr neutron activation. Due to its long half-life, 93 Zr is one of the interest radionuclides for assessment studies performance of waste storage or disposal. Measurement of 93 Zr is difficult owing to its trace level concentration and its low activity in nuclear wastes and further because its certified standards are not frequently available. The aim of this work was to apply a selective radiochemical separation methodology for 93 Zr determination in nuclear waste and analyze it by Inductively Coupled Plasma Mass Spectrometry (ICPMS). To set up the zirconium radiochemical separation procedure, a zirconium tracer solution was used in order to follow the zirconium behavior during the radiochemical separation. A tracer solution containing the main interferences, Ba, Co, Eu, Fe, Mn, Nb, Ni, Sr, and Y was used in order to verify the decontamination factor during separation process. The limit of detection of 0,039 ppb was obtained for zirconium standard solutions by ICPMS. Then, the protocol will be applied to low level waste (LLW) and intermediate level waste (ILW) from nuclear power plants. (author)

Ab initio atomic simulation of hydrogen and iodine effects in zirconium

International Nuclear Information System (INIS)

Domain, Ch.

2002-03-01

In this work we present ab initio atomic simulations concerning the effects of hydrogen and iodine in hexagonal zirconium. We first studied the point defects in the dilute Zr-H (and to a less extend Zr-H-O) systems and concluded that it is better described within the generalised gradient approximation for the exchange and correlation functional. We calculated the hydrogen thermal diffusion coefficient in solid solution that agree very well with the experimental values. The calculated formation energy of different self-interstitial configuration are rather small (around 3 eV) and close to each other indicating the high complexity of these defects. We studied the core structure of the screw dislocation that has a preferential prismatic spreading. We also calculated the gamma surface for different gliding planes. The influence of hydrogen, that induces a significant reduction of the gamma surfaces excess energies, allows to qualitatively explain experimental results regarding some hydrogen effects on hexagonal zirconium plastic deformation. We also discussed the effect of zirconium hydride stoichiometry on gamma surfaces. The results concerning the iodine and oxygen adsorption on zirconium surfaces, inducing the evaluation of the effective surface energy reduction as a function of the iodine partial pressure allow for a better description of iodine induced stress corrosion cracking of zirconium. (author)

Preparation of coherent deposits of metallic titanium and zirconium by fused salts electrolysis. Preparacion de depositos coherentes de titanio y circonio metalicos por electrolisis de sales fundidas

Energy Technology Data Exchange (ETDEWEB)

Perillo, P.M.; Botbol, J. (Comision Nacional de Energia Atomica, Departamento de Desarrollo de Procesos, Buenos Aires (Argentina))

1994-01-01

The production of coherent deposits of metallic titanium and zirconium bath composition and operating conditions were studied. The cathode was a striated iron cylinder and a graphite crucible served as anode. K[sub 2]TiF[sub 6] and K[sub 2]ZrF[sub 6] dissolved in fused NaCl at 800 degree centigree may be electrolyzed under an insert gas atmosphere. It was found that the deposits depend on the electrolytic composition of the bath while other variables in the studied values do not influence significantly. (Author) 11 refs.

Control and monitoring of the localized corrosion of zirconium in acidic chloride solutions

International Nuclear Information System (INIS)

Fahey, J.; Holmes, D.; Yau, T.L.

1995-01-01

Zirconium in acidic chloride solutions which are contaminated with ferric or cupric cations is prone to localized corrosion. This tendency can be reduced by ensuring that the zirconium surface is clean and smooth. In this paper, the effect of surface condition on the localized corrosion of zirconium in acidic chloride solutions is predicted with potentiodynamic scans. These predictions are confirmed by weight loss tests on various combinations of surface finish and acid concentrations. A real time indication of localized corrosion is seen by monitoring the electrochemical noise produced between two similar electrodes immersed in an acidic chloride solutions. Electrochemical noise monitoring correlates well with the predictions from potentiodynamic and weight loss experiments. The electrochemical noise results show that while an elevated (more anodic) potential caused by ferric ion contamination may be a necessary condition for localized corrosion, it is not a sufficient condition: A smooth, clean zirconium surface reduces the localized corrosion of zirconium

Cathodic behavior of zirconium in aqueous solutions

International Nuclear Information System (INIS)

Hine, F.; Yasuda, M.; Sato, H.

1977-01-01

The electrochemical behavior of Zr was studied by polarization measurements. The surface oxide and zirconium hydride formed by cathodic polarization of Zr have been examined by X-ray, SEM, and a hardness tester. Zirconium hydride would form on Zr cathode after the surface oxide is reduced at the potential, which is several hundred mV more noble than the predicted value shown by the Pourbaix diagram. The parameters for the hydrogen evolution reaction on the hydride formed Zr cathode differs from that on the oxide covered surface, which means that hydrogen evolution takes place on both surfaces under a different mechanism, while details are still veiled at present

Selection of a glass-ceramic formulation to immobilize fluorinel- sodium calcine

International Nuclear Information System (INIS)

Staples, B.A.; Wood, H.C.

1994-12-01

One option for immobilizing calcined high level wastes produced by nuclear fuel reprocessing activities at the Idaho Chemical Processing Plant (ICPP) is conversion to a glass-ceramic form through hot isostatic pressing. Calcines exist in several different chemical compositions, and thus candidate formulations have been developed for converting each to glass-ceramic forms which are potentially resistant to aqueous corrosion and stable enough to qualify for repository storage. Fluorinel/Na, a chemically complex calcine type, is one of the types being stored at ICPP, and development efforts have identified three formulations with potential for immobilizing it. These are a glass forming additive that uses aluminum metal to enhance reactivity, a second glass forming additive that uses titanium metal to enhance reactivity and a third that uses not only a combination of silicon and titanium metals but enough phosphorous pentoxide to form a calcium phosphate host phase in the glass-ceramic product. Glass-ceramics of each formulation performed well in restricted characterization tests. However, none of the three was subjected to rigorous testing that would provide information on whether each was processable, that is able to retain favorable characteristics over a practical range of processing conditions

Electrochemical formation of uranium-zirconium alloy in LiCl-KCl melts

Energy Technology Data Exchange (ETDEWEB)

Murakami, Tsuyoshi, E-mail: m-tsuyo@criepi.denken.or.j [Central Research Institute of Electric Power Industry (CRIEPI), Komae-shi, Tokyo 201-8511 (Japan); Kato, Tetsuya; Kurata, Masaki [Central Research Institute of Electric Power Industry (CRIEPI), Komae-shi, Tokyo 201-8511 (Japan); Yamana, Hajimu [Research Reactor Institute, Kyoto University, Kumatori-cho, Sennan-gun, Osaka 590-0494 (Japan)

2009-11-15

Since zirconium is considered an electrochemically active species under practical conditions of the electrorefining process, it is crucial to understand the electrochemical behavior of zirconium in LiCl-KCl melts containing actinide ions. In this study, the electrochemical codeposition of uranium and zirconium on a solid cathode was performed. It was found that the delta-(U, Zr) phase, which is the only intermediate phase of the uranium-zirconium binary alloy system, was deposited on a tantalum substrate by potentiostatic electrolysis at -1.60 V (vs. Ag{sup +}/Ag) in LiCl-KCl melts containing 0.13 in mol% UCl{sub 3} and 0.23 in mol% ZrCl{sub 4} at 773 K. To our knowledge, this is the first report on the electrochemical formation of the delta-(U, Zr) phase. The relative partial molar properties of uranium in the delta-(U, Zr) phase were evaluated by measuring the open-circuit-potentials of the electrochemically prepared delta-phase electrode.

Electrochemical formation of uranium-zirconium alloy in LiCl-KCl melts

International Nuclear Information System (INIS)

Murakami, Tsuyoshi; Kato, Tetsuya; Kurata, Masaki; Yamana, Hajimu

2009-01-01

Since zirconium is considered an electrochemically active species under practical conditions of the electrorefining process, it is crucial to understand the electrochemical behavior of zirconium in LiCl-KCl melts containing actinide ions. In this study, the electrochemical codeposition of uranium and zirconium on a solid cathode was performed. It was found that the δ-(U, Zr) phase, which is the only intermediate phase of the uranium-zirconium binary alloy system, was deposited on a tantalum substrate by potentiostatic electrolysis at -1.60 V (vs. Ag + /Ag) in LiCl-KCl melts containing 0.13 in mol% UCl 3 and 0.23 in mol% ZrCl 4 at 773 K. To our knowledge, this is the first report on the electrochemical formation of the δ-(U, Zr) phase. The relative partial molar properties of uranium in the δ-(U, Zr) phase were evaluated by measuring the open-circuit-potentials of the electrochemically prepared δ-phase electrode.

Arc melting in inert gas atmosphere of zirconium sponge

International Nuclear Information System (INIS)

Julio Junior, O.; Andrade, A.H.P. de

1991-01-01

The obtainment of metallic zirconium in laboratory scale with commercial and nuclear quality is the objective of the Metallurgy Department of IEN/CNEN - Brazil, so a melting procedure of zirconium sponge in laboratory scale using an arc furnace in inert atmosphere is developed. The effects of atmosphere operation, and the use of gas absorber and the sponge characteristics over the quality of button in as-cast reporting with hardness measures are described. (C.G.C.)

Structural Integrity Program for the Calcined Solids Storage Facilities at the Idaho Nuclear Technology and Engineering Center

International Nuclear Information System (INIS)

Bryant, J.W.; Nenni, J.A.

2003-01-01

This report documents the activities of the structural integrity program at the Idaho Nuclear Technology and Engineering Center relevant to the high-level waste Calcined Solids Storage Facilities and associated equipment, as required by DOE M 435.1-1, ''Radioactive Waste Management Manual.'' Based on the evaluation documented in this report, the Calcined Solids Storage Facilities are not leaking and are structurally sound for continued service. Recommendations are provided for continued monitoring of the Calcined Solids Storage Facilities

Structural Integrity Program for the Calcined Solids Storage Facilities at the Idaho Nuclear Technology and Engineering Center

International Nuclear Information System (INIS)

Jeffrey Bryant

2008-01-01

This report documents the activities of the structural integrity program at the Idaho Nuclear Technology and Engineering Center relevant to the high-level waste Calcined Solids Storage Facilities and associated equipment, as required by DOE M 435.1-1, 'Radioactive Waste Management Manual'. Based on the evaluation documented in this report, the Calcined Solids Storage Facilities are not leaking and are structurally sound for continued service. Recommendations are provided for continued monitoring of the Calcined Solids Storage Facilities

Experiments on interactions between zirconium-containing melt and water (ZREX). Hydrogen generation and chemical augmentation of energetics

Energy Technology Data Exchange (ETDEWEB)

Cho, D.H.; Armstrong, D.R.; Gunther, W.H. [Argonne National Lab., IL (United States); Basu, S.

1998-01-01

The results of the first data series of experiments on interactions between zirconium-containing melt and water are described. These experiments involved dropping 1-kg batches of pure zirconium or zirconium-zirconium dioxide mixture melt into a column of water. A total of nine tests were conducted, including four with pure zirconium melt and five with Zr-ZrO{sub 2} mixture melt. Explosions took place only in those tests which were externally triggered. While the extent of zirconium oxidation in the triggered experiments was quite extensive, the estimated explosion energetics were found to be very small compared to the combined thermal and chemical energy available. (author)

Phosphorous removal from aqueous solution can be enhanced through the calcination of lime sludge.

Science.gov (United States)

Bal Krishna, K C; Niaz, Mohamed R; Sarker, Dipok C; Jansen, Troy

2017-09-15

Water treatment plants generate an enormous amount of the sludge which is normally treated as waste. In the recent past, many investigations have been focused on developing an economical adsorbent using water treatment sludge to remove phosphorous (P) from aqueous solutions. However, the great extents of the studies have been limited in the use of alum- and iron-based sludges. This study, therefore, investigated the P removal performance of the calcined lime sludge. Calcined lime sludge at 700 °C significantly enhanced the P removal efficiency whereas marginal improvement was noted when the sludge calcined at 400 °C was tested. With increase P removal efficiency, final pH values of the solution also significantly increased. P removal efficiency of the calcined sludge decreased with increasing the initial P concentrations. However, the removal efficiency could be improved by increasing the weight of the sludge. Further analysis demonstrated that P removal trend followed both pseudo-second order and diffusion-chemisorption kinetics signifying the P removal is potentially due to a multi-mechanistic reaction in which, the process is controlled by intra-particle diffusion followed by chemisorptions. Copyright © 2017 Elsevier Ltd. All rights reserved.

Measurement of the loss on ignition of bulk calcined bauxite samples by neutron moderation

International Nuclear Information System (INIS)

Aylmer, J.A.; Borsaru, M.

1985-01-01

The production of high-grade calcined bauxite is very dependent on the moisture content of the final product. Existing procedures rely on the ignition of small samples to monitor the effectiveness of the calcination process. The results obtained by this gravimetric technique are several hours behind production and do not permit regular adjustment of the furnace to optimize the control of the chemically bound water content (LOI). To provide rapid and more relevant results, a neutron moderation technique has been developed for measuring the LOI of bulk samples of calcined bauxite while they are still hot. The method uses fast neutrons from an 241 Am-Be neutron source to irradiate the samples, and the backscattered thermal neutrons detected are a measure of bound moisture content. The rms deviation between neutron and conventional determinations of LOI, in 15 calcined bauxite samples, was 0.08 per cent LOI over the range 0.1 to 0.9 per cent LOI. When allowance is made for the rms error in the ignition method, the error in the neutron method is found to be 0.07 per cent LOI

Volatilities of ruthenium, iodine, and technetium on calcining fission product nitrate wastes

International Nuclear Information System (INIS)

Rimshaw, S.J.; Case, F.N.

1980-01-01

Various high-level nitrate wastes were subjected to formic acid denitration. Formic acid reacts with the nitrate anion to yield noncondensable, inert gases according to the following equation: 4 HCOOH + 2 HNO 3 → N 2 O + 4 CO 2 + 5 H 2 O. These gases can be scrubbed free of 106 Ru, 131 I, and 99 Tc radioactivities prior to elimination from the plant by passage through HEPA filters. The formation of deleterious NO/sub x/ is avoided. Moreover, formic acid reduces ruthenium to a lower valence state with a sharp reduction in RuO 4 volatility during subsequent calcination of the pretreated waste. It is shown that a minimum of 3% of RuO 4 in an off-gas stream reacts with Davison silica gel (Grade 40) to give a fine RuO 2 aerosol having a particle size of 0.5 μ. This RuO 2 aerosol passes through water or weak acid scrub solutions but is trapped by a caustic scrub solution. Iodine volatilizes almost completely on calcining an acidic waste, and the iodine volatility increases with increasing calcination temperature. On calcining an alkaline sodium nitrate waste the iodine volatility is about an order of magnitude lower, with a relatively low iodine volatility of 0.39% at a calcination temperature of 250 0 C and a moderate volatility of 9.5% at 600 0 C. Volatilities of 99 Tc were generally 0 C. Data are presented to indicate that 99 Tc concentrates in the alkaline sodium nitrate supernatant waste, with approx. 10 mg 99 Tc being associated with each curie of 137 Cs present in the waste. It is shown that lutidine (2,4 dimethyl-pyridine) extracts Tc(VII) quantitatively from alkaline supernatant wastes. The distribution coefficient (K/sub D/) for Tc(VII) going into the organic phase in the above system is 102 for a simulated West Valley waste and 191 for a simulated Savannah River Plant (SRP) waste

Hydrolysis of TBF and TiAP in presence of zirconium

International Nuclear Information System (INIS)

Vladimirova, M.V.; Kulikov, I.A.; Kuprij, A.A.

1992-01-01

Acid hydrolysis of organic solutions of tributyl phosphate (TBP) and tri-iso-amylphosphate (TiAP) in n-paraffin diluent in the presence of zirconium (0.025-0.1 mole/l) at nitric acid concentration of 0.3-1 mole/l is studied. Hydrolysis of extractants in a two-phase system, modelling conditions of spent fuel reprocessing and consisting of 1.1 mole/l TAP, 3 mole/l nitric acid at zirconium concentration in water phase 0.05-0.11 mole/l, at water-organic phase ratio 10:1 and at 60 deg C is also studied. Constants of TAP hydrolysis in organic and water phases are determined. Mechanism of increasing the TAP hydrolysis rate in zirconium presence is discussed. 5 refs., 2 figs., 5 tabs

Efficient One-Pot Synthesis of Colloidal Zirconium Oxide Nanoparticles for High-Refractive-Index Nanocomposites.

Science.gov (United States)

Liu, Chao; Hajagos, Tibor Jacob; Chen, Dustin; Chen, Yi; Kishpaugh, David; Pei, Qibing

2016-02-01

Zirconium oxide nanoparticles are promising candidates for optical engineering, photocatalysis, and high-κ dielectrics. However, reported synthetic methods for the colloidal zirconium oxide nanoparticles use unstable alkoxide precursors and have various other drawbacks, limiting their wide application. Here, we report a facile one-pot method for the synthesis of colloidally stable zirconium oxide nanoparticles. Using a simple solution of zirconium trifluoroacetate in oleylamine, highly stable zirconium oxide nanoparticles have been synthesized with high yield, following a proposed amidization-assisted sol-gel mechanism. The nanoparticles can be readily dispersed in nonpolar solvents, forming a long-term stable transparent solution, which can be further used to fabricate high-refractive-index nanocomposites in both monolith and thin-film forms. In addition, the same method has also been extended to the synthesis of titanium oxide nanoparticles, demonstrating its general applicability to all group IVB metal oxide nanoparticles.

Design and performance of atomizing nozzles for spray calcination of high-level wastes

International Nuclear Information System (INIS)

Miller, F.A.; Stout, L.A.

1981-05-01

A key aspect of high-level liquid-waste spray calcination is waste-feed atomization by using air atomizing nozzles. Atomization substantially increases the heat transfer area of the waste solution, which enhances rapid drying. Experience from the spray-calciner operations has demonstrated that nozzle flow conditions that produce 70-μ median-volume-diameter or smaller spray droplets are required for small-scale spray calciners (drying capacity less than 80 L/h). For large-scale calciners (drying capacity greater than 300 L/h), nozzle flow conditions that produce 100-μ median-volume-diameter or smaller spray droplets are required. Mass flow ratios of 0.2 to 0.4, depending on nozzle size, are required for proper operation of internal-mix atomizing nozzles. Both internal-mix and external-mix nozzles have been tested at PNL. Due to the lower airflow requirements and fewer large droplets produced, the internal-mix nozzle has been chosen for primary development in the spray calciner program at PNL. Several nozzle air-cap materials for internal-mix nozzles have been tested for wear resistance. Results show that nozzle air caps of stainless steel and Cer-vit (a machineable glass ceramic) are suceptible to rapid wear by abrasive slurries, whereas air caps of alumina and reaction-bonded silicon nitride show only slow wear. Longer-term testing is necessary to determine more accurately the actual frequency of nozzle replacement. Atomizing nozzle air caps of alumina are subject to fracture from thermal shock, whereas air caps of silicon nitride and Cer-vit are not. Fractured nozzles are held in place by the air-cap retaining ring and continue to atomize satisfactorily. Therefore, fractures caused by thermal shocking do not necessarily result in nozzle failure

Interim status of vertical calciner testing through calendar year 1996

International Nuclear Information System (INIS)

Compton, J.A.

1998-01-01

A prototype vertical calciner was constructed and tested for use in converting plutonium solutions to dry plutonium dioxide in the Hanford Plutonium Finishing Plant. Six non-radioactive runs were completed in June and July, 1995. Fourteen runs with plutonium nitrate solutions were completed between September, 1995 and August, 1996. Equipment modifications were made following those runs. The test runs with plutonium have converted 62.3 L of feed solution containing 11.1 kg of plutonium into dry plutonium dioxide containing 8.5 kg of plutonium. The decrease in product plutonium content is primarily due to plutonium accumulation within the calciner powder bed from particle compaction. Nine of the eleven product batches have had Losses On Ignition that met the storage criterion of less than 0.5 weight percent at 950 C. The highest Loss On Ignition found was 0.718 weight percent. Initial problems with agitator shaft binding and breakage of bushings have been eliminated. A feed pump control problem has been found and the pump replaced. Improvement in scrubber efficiency is needed. Future runs are planned to confirm that (1) the remainder of product meets the Loss On Ignition criterion, (2) the replacement feedpump works as needed, and (3) the scrubber efficiency improves. The operating staff for the production calciner may also be observing the prototype's runs to gain familiarity with the process and equipment

Titanium and zirconium alloys

International Nuclear Information System (INIS)

Pinard Legry, G.

1994-01-01

Titanium and zirconium pure and base alloys are protected by an oxide film with anionic vacancies which gives a very good resistance to corrosion in oxidizing medium, in some ph ranges. Results of pitting and crevice corrosion are given for Cl - , Br - , I - ions concentration with temperature and ph dependence, also with oxygenated ions effect. (A.B.). 32 refs., 6 figs., 3 tabs

Design and development of novel MRI compatible zirconium- ruthenium alloys with ultralow magnetic susceptibility.

Science.gov (United States)

Li, H F; Zhou, F Y; Li, L; Zheng, Y F

2016-04-19

In the present study, novel MRI compatible zirconium-ruthenium alloys with ultralow magnetic susceptibility were developed for biomedical and therapeutic devices under MRI diagnostics environments. The results demonstrated that alloying with ruthenium into pure zirconium would significantly increase the strength and hardness properties. The corrosion resistance of zirconium-ruthenium alloys increased significantly. High cell viability could be found and healthy cell morphology observed when culturing MG 63 osteoblast-like cells and L-929 fibroblast cells with zirconium-ruthenium alloys, whereas the hemolysis rates of zirconium-ruthenium alloys are zirconium-ruthenium alloys (1.25 × 10(-6) cm(3)·g(-1)-1.29 × 10(-6) cm(3)·g(-1) for zirconium-ruthenium alloys) are ultralow, about one-third that of Ti-based alloys (Ti-6Al-4V, ~3.5 × 10(-6) cm(3)·g(-1), CP Ti and Ti-6Al-7Nb, ~3.0 × 10(-6) cm(3)·g(-1)), and one-sixth that of Co-Cr alloys (Co-Cr-Mo, ~7.7 × 10(-6) cm(3)·g(-1)). Among the Zr-Ru alloy series, Zr-1Ru demonstrates enhanced mechanical properties, excellent corrosion resistance and cell viability with lowest magnetic susceptibility, and thus is the optimal Zr-Ru alloy system as therapeutic devices under MRI diagnostics environments.

Zirconium Phosphate Supported MOF Nanoplatelets.

Science.gov (United States)

Kan, Yuwei; Clearfield, Abraham

2016-06-06

We report a rare example of the preparation of HKUST-1 metal-organic framework nanoplatelets through a step-by-step seeding procedure. Sodium ion exchanged zirconium phosphate, NaZrP, nanoplatelets were judiciously selected as support for layer-by-layer (LBL) assembly of Cu(II) and benzene-1,3,5-tricarboxylic acid (H3BTC) linkers. The first layer of Cu(II) is attached to the surface of zirconium phosphate through covalent interaction. The successive LBL growth of HKUST-1 film is then realized by soaking the NaZrP nanoplatelets in ethanolic solutions of cupric acetate and H3BTC, respectively. The amount of assembled HKUST-1 can be readily controlled by varying the number of growth cycles, which was characterized by powder X-ray diffraction and gas adsorption analyses. The successful construction of HKUST-1 on NaZrP was also supported by its catalytic performance for the oxidation of cyclohexene.

Effect of calcination conditions of pork bone sludge on behaviour

Indian Academy of Sciences (India)

... bone sludge from meat plant via two essentially different calcination methods using ... tissue and suitability for further investigations intended for medical grafting. ... The Alfred Meissner Higher School of Dental Engineering and Humanities, ...

Improvement of the crystallinity and photocatalytic property of zinc oxide as calcination product of Zn–Al layered double hydroxide

International Nuclear Information System (INIS)

Ahmed, Abdullah Ahmed Ali; Talib, Zainal Abidin; Hussein, Mohd Zobir bin; Zakaria, Azmi

2012-01-01

Highlights: ► ZnO phase and ZnAl 2 O 4 spinel can be formed as Zn–Al–NO 3 –LDH calcination products. ► The crystallinity of ZnO phase increased with an increase of calcination temperature. ► The optical band gaps of ZnO were improved with an increase in temperature. ► The oxygen vacancies in ZnO and ZnAl 2 O 4 generated the ESR signals. - Abstract: Zinc oxide with different degrees of crystallinity can be formed as Zn–Al-layered double hydroxide (Zn–Al–NO 3 –LDH) calcination products. ZnAl 2 O 4 spinel is also formed in a range of calcination temperatures from 600 to 1000 °C from the LDH. X-ray diffraction patterns showed that the crystallinity of the ZnO phase increased as calcination temperatures increased. The LDH structure was fully collapsed at and above 400 °C. The photocatalytic activity was determined by UV–VIS–NIR diffuse reflectance spectroscopy. The band gap of the calcined samples increased as the calcination temperature increased. Electron spin resonance (ESR) spectra of the fresh and calcined LDH at room temperature demonstrated that oxygen vacancies in the ZnO and ZnAl 2 O 4 were responsible for the generation of ESR signals. One BET specific surface area increased from 1 m 2 /g for the LDH to a maximum at 400 °C (43 m 2 /g) and decreased thereafter down to 6 m 2 /g at 1000 °C.

Adsorption of zirconium from nitric acid solutions on hydrated tin dioxide

Energy Technology Data Exchange (ETDEWEB)

Tret' yakov, S Ya; Sharygin, L M; Egorov, Yu V

1977-01-01

Adsorption of zirconium from nitric acid solutions has been studied with the use of the labeled atom method on hydrated tin dioxide depending on the sorbate concentration, pH and prehistory of the solution. It has been found that adsorption behavior of zirconium essentially depends on its state in the solution.

A Summary of Properties Used to Evaluate INEEL Calcine Disposal in the Yucca Mountain Repository

International Nuclear Information System (INIS)

Dahl, C.A.

2003-01-01

To support evaluations of the direct disposal of Idaho National Engineering and Environmental Laboratory calcines to the repository at Yucca Mountain, an evaluation of the performance of the calcine in the repository environment must be performed. This type of evaluation demonstrates, through computer modeling and analysis, the impact the calcine would have on the ability of the repository to perform its function of containment of materials during the repository lifetime. This report discusses parameters that were used in the scoping evaluation conducted in FY 2003. It provides nominal values for the parameters, with explanation of the source of the values, and how the values were modified for use in repository analysis activities

Characterization of norm sources in petroleum coke calcining processes - 16314

International Nuclear Information System (INIS)

Hamilton, Ian S.; Halter, Donald A.; Fruchtnicht, Erich H.; Arno, Matthew G.; Haumann, Donald F

2009-01-01

Petroleum coke, or 'petcoke', is a waste by-product of the oil refining industry. The majority of petcoke consumption is in energy applications; catalyst coke is used as refinery fuel, anode coke for electricity conduction, and marketable coke for heating cement kilns. Roskill has predicted that long-term growth in petroleum coke production will be maintained, and may continue to increase slightly through 2012. Petcoke must first be calcined to drive off any undesirable petroleum by-products that would shorten the coke product life cycle. As an example, the calcining process can take place in large, rotary kilns heated to maximum temperatures as high as approximately 1400-1540 deg. C. The kilns and combustion/settling chambers, as well as some cooler units, are insulated with refractory bricks and other, interstitial materials, e.g., castable refractory materials, to improve the efficiency of the calcining process. The bricks are typically made of 70-85-percent bauxite, and are slowly worn away by the calcining process; bricks used to line the combustion chambers wear away, as well, but at a slower rate. It has been recognized that the refractory materials contain slight amounts of naturally occurring radioactive materials (NORM) from the uranium- and thorium-decay series. Similarly, low levels of NORM could be present in the petcoke feed stock given the nature of its origin. Neither the petcoke nor the refractory bricks represent appreciable sources of radiation or radioactive waste. However, some of the demolished bricks that have been removed from service because of the aforementioned wearing process have caused portal alarms to activate at municipal disposal facilities. This has lead to the current investigation into whether there is a NORM concentrating mechanism facilitated by the presence of the slightly radioactive feed stock in the presence of the slightly radioactive refractory materials, at calcining-zone temperatures. Research conducted to date has been

Superconductivity in zirconium-rhodium alloys

Science.gov (United States)

Zegler, S. T.

1969-01-01

Metallographic studies and transition temperature measurements were made with isothermally annealed and water-quenched zirconium-rhodium alloys. The results clarify both the solid-state phase relations at the Zr-rich end of the Zr-Rh alloy system and the influence upon the superconducting transition temperature of structure and composition.

Recovery of zirconium from pickling solution, regeneration and its reuse

Energy Technology Data Exchange (ETDEWEB)

Bhattacharjee, D. [Nuclear Fuel Complex, Hyderabad 500062 (India); Mandal, D., E-mail: dmandal10@gmail.com [Alkali Material & Metal Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Visweswara Rao, R.V.R.L.; Sairam, S.; Thakur, S. [Nuclear Fuel Complex, Hyderabad 500062 (India)

2017-05-15

Graphical abstract: The following compares the performance of fresh pickling solution (PS) and regenerated and used pickling solution (UPS). - Highlights: • Pickling of zircaloy tubes and appendages is carried out to remove oxide layer. • The pickling solution become saturated with zirconium due to reuse. • As NaNO{sub 3} concentration increases, conc. of Zr in pickling solution decreases. • Experimental results shows that, used pickling solution can be regenerated. • Regenerated solution may be reused by adding makeup quantities of HF-HNO{sub 3}. - Abstract: The pressurized heavy water reactors use natural uranium oxide (UO{sub 2}) as fuel and uses cladding material made up of zircaloy, an alloy of zirconium. Pickling of zircaloy tubes and appendages viz., spacer and bearing pads is carried out to remove the oxide layer and surface contaminants, if present. Pickling solution, after use for many cycles i.e., used pickling solution (UPS) is sold out to vendors, basically for its zirconium value. UPS, containing a relatively small concentration of hydrofluoric acid. After repeated use, pickling solution become saturated with zirconium fluoride complex and is treated by adding sodium nitrate to precipitate sodium hexafluro-zirconate. The remaining solution can be recycled after suitable makeup for further pickling use. The revenue lost by selling UPS is very high compared to its zirconium value, which causes monetary loss to the processing unit. Experiments were conducted to regenerate and reuse UPS which will save a good amount of revenue and also protect the environment. Experimental details and results are discussed in this paper.

Talc-silicon glass-ceramic waste forms for immobilization of high- level calcined waste

International Nuclear Information System (INIS)

Vinjamuri, K.

1993-06-01

Talc-silicon glass-ceramic waste forms are being evaluated as candidates for immobilization of the high level calcined waste stored onsite at the Idaho Chemical Processing Plant. These glass-ceramic waste forms were prepared by hot isostatically pressing a mixture of simulated nonradioactive high level calcined waste, talc, silicon and aluminum metal additives. The waste forms were characterized for density, chemical durability, and glass and crystalline phase compositions. The results indicate improved density and chemical durability as the silicon content is increased

In situ Investigation of Oxide Films on Zirconium Alloy in PWR Primary Water Chemistry

Energy Technology Data Exchange (ETDEWEB)

Kim, Taeho; Choi, Kyoung Joon; Yoo, Seung Chang; Kim, Ji Hyun [Ulsan National Institute of Science and Technology, Ulsan (Korea, Republic of)

2015-05-15

Zirconium alloys are used as fuel cladding materials in nuclear power reactors, because these materials have a very low thermal neutron capture cross section as well as desirable mechanical properties. However, the Fukushima accident shows that the oxidation behavior of zirconium alloy is an important issue because the zirconium alloy functions as a shield of nuclear material (i.e., uranium, fission gas), and the degradation on zirconium cladding directly causes severe accident on nuclear power plant. Therefore, to ensure the safety of nuclear power reactors, the performance and sustainability of nuclear fuel should be understood. Currently, the water-metal interface is regarded as the rate-controlling site governing the rapid oxidation transition in high-burn-up fuels. Zirconium oxide is formed at the water-metal interface, and its structure and phase play an important role in determining its mechanical properties. In the early stage of the oxidation process, zirconium oxide with both tetragonal and monoclinic phases is formed. With an increase in the oxidation time to 150 h, the unstable tetragonal phase disappears and the monoclinic phase is dominant and possibly because of the stress relaxation according to previous and present results.

Amine extraction of lead(II) and zirconium(IV) with succinate media

International Nuclear Information System (INIS)

Mahamuni, S.V.; Mane, C.P.; Sargar, B.M.; Rajmane, M.M.; Anuse, M.A.

2004-01-01

Lead is an important constituent of various alloys, which are in increasing demand in manufacture of batteries and nuclear shielding while the use of zirconium in nuclear power plants as entirely cladding uranium fuel is most important. This study was carried out to optimize the extraction conditions for Pb(II) and zirconium(IV)

Reaction of hydrogen peroxide with uranium zirconium oxide solid solution - Zirconium hinders oxidative uranium dissolution

Science.gov (United States)

Kumagai, Yuta; Takano, Masahide; Watanabe, Masayuki

2017-12-01

We studied oxidative dissolution of uranium and zirconium oxide [(U,Zr)O2] in aqueous H2O2 solution to estimate (U,Zr)O2 stability to interfacial reactions with H2O2. Studies on the interfacial reactions are essential for anticipating how a (U,Zr)O2-based molten fuel may chemically degrade after a severe accident. The fuel's high radioactivity induces water radiolysis and continuous H2O2 generation. Subsequent reaction of the fuel with H2O2 may oxidize the fuel surface and facilitate U dissolution. We conducted our experiments with (U,Zr)O2 powder (comprising Zr:U mole ratios of 25:75, 40:60, and 50:50) and quantitated the H2O2 reaction via dissolved U and H2O2 concentrations. Although (U,Zr)O2 reacted more quickly than UO2, the dissolution yield relative to H2O2 consumption was far less for (U,Zr)O2 compared to that of UO2. The reaction kinetics indicates that most of the H2O2 catalytically decomposed to O2 at the surface of (U,Zr)O2. We confirmed the H2O2 catalytic decomposition via O2 production (quantitative stoichiometric agreement). In addition, post-reaction Raman scattering spectra of the undissolved (U,Zr)O2 showed no additional peaks (indicating a lack of secondary phase formation). The (U,Zr)O2 matrix is much more stable than UO2 against H2O2-induced oxidative dissolution. Our findings will improve understanding on the molten fuels and provide an insight into decommissioning activities after a severe accident.

Phyto-availability of zirconium in relation with initial speciation, solubility and soil characteristics

International Nuclear Information System (INIS)

Ferrand, E.; Benedetti, M.; Dumat, C.; Ferrand, E.; Leclerc-Cessac, E.

2005-01-01

During the last decades, the use of zirconium in industry has been widely developed and there is a potential risk of zirconium contamination. The long half-life isotope 93 Zr (T1/2=10 6 years) is largely observed in radioactive wastes. Therefore, the long-term prediction of the zirconium fate in the environment is essential. Due to its low solubility and strong tendency to polymerize, zirconium is usually considered as immobile, however the evidence of Zr mobility in certain conditions such as tropical weathering has been demonstrated. Soil-plant transfer is an important link in the chain of events which leads to radionuclide entry into the human food chain, but only few studies concern the Zr transfer to plants. The primary aim of this investigation is to verify if zirconium can be absorbed by edible plants (young peas and tomatoes) and to study the influence of Zr speciation on its availability. The second aim is to highlight the potential influence of plants on the Zr solubility in soil from the measurements of K d and with chemical extractions. Two agricultural top soils closed to the underground experimental laboratory (Meuse/Haute Marne, France) of the French National Agency for management of radioactive wastes (ANDRA) were collected: a sandy clayey loamy soil (A) and a clayey calcareous soil (B). The main differences between the two soils are: the pH, the texture and the carbonate content. In order to investigate the influence of the Zr speciation on its plant availability, soils were spiked with different forms of Zr chosen for their natural occurrence in the environment. Soil adsorption of Zr in batch experiments was realized (various initial [Zr], pH and I) in order to determine adsorption isotherms and partition coefficients (K d ). Tomatoes and peas were exposed to Zr by contact with the various soils during 8 days. After acidic digestion of the dried roots and aerial parts, the total Zr concentrations were measured by a quadrupole ICP-MS spectrometer

A parametric study of a solar calcinator using computational fluid dynamics

International Nuclear Information System (INIS)

Fidaros, D.K.; Baxevanou, C.A.; Vlachos, N.S.

2007-01-01

In this work a horizontal rotating solar calcinator is studied numerically using computational fluid dynamics. The specific solar reactor is a 10 kW model designed and used for efficiency studies. The numerical model is based on the solution of the Navier-Stokes equations for the gas flow, and on Lagrangean dynamics for the discrete particles. All necessary mathematical models were developed and incorporated into a computational fluid dynamics model with the influence of turbulence simulated by a two-equation (RNG k-ε) model. The efficiency of the reactor was calculated for different thermal inputs, feed rates, rotational speeds and particle diameters. The numerically computed degrees of calcination compared well with equivalent experimental results

Effect of calcination temperature on the synthesis of potassium titanate with platy morphology

International Nuclear Information System (INIS)

Farina, R.; Fredericci, C.; Yoshimura, H.N.

2011-01-01

The dramatic increases in the number of pneumoconiosis cases have stimulated the search of new materials for replacement of asbestos fibers. Titanate plates with formula A y Ti 2-x M x O 4 , where A = K, Rb, Cs and M = Li, Mg, Co, Ni, Cu, Zn, Mn (III), Fe (III) have been studied as an alternative for the use of fibers. The effect of the variation of calcination temperature on the reaction of K 2 CO 3 -TiO 2 -Mg(OH) 2 system was studied with the aim of understanding the relationship of this parameter with the morphology and symmetry of the obtained plates. For this study the samples were calcined for 5 hours at temperatures of 950°C, 1000°C, 1050°C and 1100°C. The powders were analyzed by X-ray diffraction and scanning electron microscopy. It was concluded that 1000°C is the better calcination temperature for obtaining more symmetric plates with smaller particle size dispersion. (author)

On composition and thermal degradation of basic zirconium sulfates

Energy Technology Data Exchange (ETDEWEB)

Grizik, A A; Nekhamkin, L G; Kondrashova, I A; Serebrennikov, E L; Kerina, V P

1988-02-01

Methods of potentiometric titration, conductometry and thermal gravimetric analysis are used to study composition and properties of basic zirconium sulfates (BZS) obtained under different conditions of precipitation from aqueous solutions. Three X-ray amorphous phases of BZR with mole ratio SO/sub 4//sup 2-/:Zr, being 0.60+-0.03; 0.37+-0.04 and 0.176+-0.005, are identified. Different character of thermal decomposition of these phases in the process of zirconium dioxide preparation from BZS is confirmed.

On composition and thermal degradation of basic zirconium sulfates

International Nuclear Information System (INIS)

Grizik, A.A.; Nekhamkin, L.G.; Kondrashova, I.A.; Serebrennikov, E.L.; Kerina, V.P.

1988-01-01

Methods of potentiometric titration, conductometry and thermal gravimetric analysis are used to study composition and properties of basic zirconium sulfates (BZS) obtained under different conditions of precipitation from aqueous solutions. Three X-ray amorphous phases of BZR with mole ratio SO 4 2- :Zr, being 0.60±0.03; 0.37±0.04 and 0.176±0.005, are identified. Different character of thermal decomposition of these phases in the process of zirconium dioxide preparation from BZS is confirmed

Zirconium molybdate hydrate precipitates in spent nuclear fuel reprocessing

International Nuclear Information System (INIS)

Magnaldo, A.; Noire, M.H.; Esbelin, E.; Dancausse, J.P.; Picart, S.

2004-01-01

This paper presents through 2 posters a general overview studies realised by CEA teams on deposits observed in the La Hague plant dissolution facilities. Their main constituents are metallic debris bound together with zirconium molybdate hydrate. A comprehensive study of zirconium molybdate hydrate formation included nucleation and growth kinetics was developed. Fouling mechanisms were consequently explained as influenced by the operation conditions. Pu insertion was also overviewed. Its behaviour is important when curative and preventive chemical treatments are considered. (authors)

Zirconium microstructures: uncharted possibilities

International Nuclear Information System (INIS)

Samajdar, I.; Kumar, Gulshan; Singh, Jaiveer; Lodh, Arijit; Srivastava, D.; Tewari, R.; Dey, G.K.; Saibaba, N.

2015-01-01

The 'conventional' Zirconium microstructures can be significantly extended with information on: (i) microtexture, (ii) residual stresses and (iii) local mechanical properties. Though these involve different tools, but a consolidated microstructure can be crated. This is the theme of this presentation. Examples of this consolidated picture will be made from deformation twinning, recovery-recrystallization, burst ductility and orientation versus solid solution hardening. (author)

Temperature dependence of lattice parameters of alpha-zirconium

International Nuclear Information System (INIS)

Versaci, R.A.; Ipohorski, M.

1991-01-01

This work presents a brief review of X-ray and thermal expansion determination of lattice parameters for α-Zirconium. Data reported by different authors cover almost all the field of existence of the hexagonal phase of Zirconium, from temperatures as low as 4.2 K up to about 1130 K, near the α→β transformation temperature. Polynomial expressions based on a least squares fitting of experimental data are also presented. The expressions obtained by Goldak et al. are considered to be the most complete. The influence of impurities on the lattice parameters is also discussed. (Author) [es

A contribution to the study of arc melting in inert gas atmospheres of zirconium sponge

International Nuclear Information System (INIS)

Julio Junior, O.

1990-01-01

Mettalic zirconium is a material of great interest in the nuclear industry due to its low thermal neutron cross section, high strength and corrosion resistance. The latter permits its use in the chemical industry. In this study, a critical bibliographic revision of the industrial processes used for the melting and consolidation of zirconium sponge has been carried out. A procedure for the melting of zirconium on a laboratory scale, has been established. An nonconsumable-electrode arc furnace have been used. The effect of process variables like atmosphere, melting current and getter, have been showed. The influence of sponge characteristics on the qualities of cast zirconium buttons have been studied. The present study is a contribution towards future investigations to obtain high purity cast zirconium and its alloys commercially known as zircaloy. (author)

Design and development of novel MRI compatible zirconium- ruthenium alloys with ultralow magnetic susceptibility

Science.gov (United States)

Li, H.F.; Zhou, F.Y.; Li, L.; Zheng, Y.F.

2016-01-01

In the present study, novel MRI compatible zirconium-ruthenium alloys with ultralow magnetic susceptibility were developed for biomedical and therapeutic devices under MRI diagnostics environments. The results demonstrated that alloying with ruthenium into pure zirconium would significantly increase the strength and hardness properties. The corrosion resistance of zirconium-ruthenium alloys increased significantly. High cell viability could be found and healthy cell morphology observed when culturing MG 63 osteoblast-like cells and L-929 fibroblast cells with zirconium-ruthenium alloys, whereas the hemolysis rates of zirconium-ruthenium alloys are alloys and Ti-based alloys, the magnetic susceptibilities of the zirconium-ruthenium alloys (1.25 × 10−6 cm3·g−1–1.29 × 10−6 cm3·g−1 for zirconium-ruthenium alloys) are ultralow, about one-third that of Ti-based alloys (Ti–6Al–4V, ~3.5 × 10−6 cm3·g−1, CP Ti and Ti–6Al–7Nb, ~3.0 × 10−6 cm3·g−1), and one-sixth that of Co–Cr alloys (Co–Cr–Mo, ~7.7 × 10−6 cm3·g−1). Among the Zr–Ru alloy series, Zr–1Ru demonstrates enhanced mechanical properties, excellent corrosion resistance and cell viability with lowest magnetic susceptibility, and thus is the optimal Zr–Ru alloy system as therapeutic devices under MRI diagnostics environments. PMID:27090955

Study of solution speciation, soil retention and soil-plant transfer of zirconium

International Nuclear Information System (INIS)

Ferrand, E.

2005-12-01

Within the framework of the risks prevention policy of Andra, the radioactive zirconium introduction ( 93 Zr and 95 Zr) into the environment could be carried out starting from the nuclear waste whose storage is envisaged in deep geological layers. Thus, the goal of this study was to evaluate the parameters and phenomena influencing speciation (various chemical forms) and the soil-plant transfer of zirconium. Experiments of adsorption/desorption of zirconium with different ligands likely to be present in soils (goethite and humic acid) and with two soils, with contrasted characteristics, close to the underground research laboratory of Andra (Meuse) were carried out. These results of adsorption were then confronted with those obtained by the MUSIC and NICA-DONNAN models carried out using the computer code ECOSAT. Zr presents a strong affinity for the two types of soils and the soils constituents. Specific interactions of internal sphere type with the goethite were highlighted using the model. Soil-solution partition coefficients, or K d , values increase with pH and contact time. Various types of edible plants, pea (Pisum sativum L.) and tomato (Lycopersicon esculentum L cv. St Pierre) were cultivated in hydroponic conditions and in soils spiked with various sources of Zirconium. The maximum zirconium contents are mainly measured in the roots of the plants. The soil-plant transfer factors measured during these experiments show a weak bioavailability of zirconium. An influence of speciation on Zr bioavailability is however highlighted. Some chemical forms, such as oxychloride or acetate, are more easily mobilized than others by the plant. (author)

Preparation of zirconium molybdate gel for 99mTc gel generator

International Nuclear Information System (INIS)

Aliludin, Z.; Ohkubo, Masatake; Kushita, Kouhei

1988-09-01

Zirconium molybdate gel has excellent characteristics for use as column matrix material of 99m Tc generators. In this work, zirconium molybdate gels were prepared under different conditions; pH's of molybdate solutions from 2.5 to 7.0, Mo:Zr molar ratios from 0.7:1.0 to 1.3:1.0, drying temperatures from an ambient temperature to 200 deg C, and drying times from 1 h to 25 h. Contents of water, nitrate, molybdenum and zirconium were measured to examine the fundamental conditions in gel preparation. The Mo:Zr molar ratio was 1.0:1.0 for the most of gels obtained. A 99m Tc generator was prepared with an amorphous zirconium molybdate containing a tracer level of 99 Mo as column matrix material. Elution of 99m Tc was rapid and the average elution efficiency was 90 % for 6 ml elutions. Contents of radionuclidic impurities, Zr and Mo in the eluates, were low enough to meet the pharmacopoeia requirements for human use. (author)

Mobile calcination and cementation unit for solidification of concentrated radioactive wastes

International Nuclear Information System (INIS)

Napravnik, J.; Sazavsky, P.; Skaba, V.; Skvarenina, R.; Ditl, P.

1985-01-01

Mobile experimental unit MESA-1 was developed and manufactured for processing radioactive concentrates by direct cementation. The unit is mainly designed for processing low-level liquid wastes from nuclear power plants and other nuclear installations, in which the level of radioactivity does not exceed 10 10 Bq/m 3 , the salt content of liquid solutions does not exceed 500 kg/m 3 and the maximum amount of boric acid is 130 kg/m 3 . The equipment is built into three modules which may be assembled and dismantled in a short time and transported separately. The unit without the calciner module was tested in non-radioactive mode and in operation with actual radioactive wastes from the V-1 nuclear power plant. The course and results of the tests are described in detail. All project design values were achieved, a total of 18 dm 3 model solutions were processed and 1 m 3 of actual wastes with a salt content of 450 kg/m 3 . The test showed that with regard to the radiation level reached it will be necessary in the process of calcination to increase the shielding of certain exposed points. The calciner module is being assembled for completion. (Z.M.)

Influence of calcined mud on the mechanical properties and shrinkage of self-compacting concrete

Directory of Open Access Journals (Sweden)

Fatima Taieb

2018-01-01

Full Text Available The use of SCC has a particular interest in terms of sustainable development. Indeed, their specific formulation leads to a greater volume of dough than for common concretes, thus, a larger quantity of cement. However, for economical, ecological and technical reasons, it is sought to limit their cement content [1]. It is therefore necessary to almost always use mineral additions as a partial replacement for cement because the technology of self-compacting concretes can consume large quantities of fines, in this case calcinated mud issued from dams dredging sediments that can give and/or ameliorate characteristics and performances of this type of concretes. Four SCCs had been formulated from the same composition where the only percentage of calcinated mud of Chorfa (west of Algeria dam changed (0%, 10%, 20% and 30%. The effect of calcinated mud on characteristics at fresh state of SCC according to AFGC was quantified. Mechanical strengths and shrinkage deformation (total, autogenous, drying were evaluated. The results show the possibility to make SCCs with different dosages of calcinated mud having strengths that can defy those of the control SCC. The analysis of free deformations indicates the beneficial impact of the mud by contributing to decrease the amplitudes of the shrinkage compared to those of the control SCC.

Plastic deformation of particles of zirconium and titanium carbide subjected to vibration grinding

Energy Technology Data Exchange (ETDEWEB)

Kravchik, A.E.; Neshpor, V.S.; Savel' ev, G.A.; Ordan' yan, S.S.

1976-12-01

A study is made of the influence of stoichiometry on the characteristics of microplastic deformation in powders of zirconium and titanium carbide subjected to vibration grinding. The carbide powders were produced by direct synthesis from the pure materials: metallic titanium and zirconium and acetylene black. As to the nature of their elastic deformation, zirconium and titanium carbides can be considered elastic-isotropic materials. During vibration grinding, the primary fracture planes are the (110) planes. Carbides of nonstoichiometric composition are more brittle.

Zirconium phosphate waste forms for low-temperature stabilization of cesium-137-containing waste streams

International Nuclear Information System (INIS)

Singh, D.; Wagh, A.S.; Tlustochowicz.

1996-04-01

Novel chemically bonded phosphate ceramics are being developed and fabricated for low-temperature stabilization and solidification of waste streams that are not amenable to conventional high-temperature stabilization processes because volatiles are present in the wastes. A composite of zirconium-magnesium phosphate has been developed and shown to stabilize ash waste contaminated with a radioactive surrogate of 137 Cs. Excellent retainment of cesium in the phosphate matrix system was observed in Toxicity Characteristic Leaching Procedure tests. This was attributed to the capture of cesium in the layered zirconium phosphate structure by intercalation ion-exchange reaction. But because zirconium phosphate has low strength, a novel zirconium/magnesium phosphate composite waste form system was developed. The performance of these final waste forms, as indicated by compression strength and durability in aqueous environments, satisfy the regulatory criteria. Test results indicate that zirconium-magnesium-phosphate-based final waste forms present a viable technology for treatment and solidification of cesium-contaminated wastes

Effect of nitrogen flow ratio on structure and properties of zirconium ...

Indian Academy of Sciences (India)

Abstract. In this study, zirconium nitride thin films were deposited on Si substrates by ion beam sputtering (IBS). Influence of N2/(N2+Ar) on the structural and physical properties of the films has been investigated with respect to the atomic ratio between nitrogen and zirconium. It was found that the thickness of layers ...

Fretting wear behavior of zirconium alloy in B-Li water at 300 °C

Science.gov (United States)

Zhang, Lefu; Lai, Ping; Liu, Qingdong; Zeng, Qifeng; Lu, Junqiang; Guo, Xianglong

2018-02-01

The tangential fretting wear of three kinds of zirconium alloys tube mated with 304 stainless steel (SS) plate was investigated. The tests were conducted in an autoclave containing 300 °C pressurized B-Li water for tube-on-plate contact configuration. The worn surfaces were examined with scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and 3D microscopy. The cross-section of wear scar was examined with transmission electron microscope (TEM). The results indicated that the dominant wear mechanism of zirconium alloys in this test condition was delamination and oxidation. The oxide layer on the fretted area consists of outer oxide layer composed of iron oxide and zirconium oxide and inner oxide layer composed of zirconium oxide.

Studies on inorganic exchanger: zirconium antimonate

International Nuclear Information System (INIS)

Dash, A.; Balasubramanian, K.R.

1992-01-01

The inorganic exchanger zirconium antimonate has been prepared and its characteristics evaluated. A method has been developed for the separation of 90 Sr and 144 Ce from fission products solution using this exchanger. (author). 23 refs., 18 f igs., 9 tabs

Pressure of saturated vapor of yttrium and zirconium acetylacetonates

Energy Technology Data Exchange (ETDEWEB)

Trembovetskij, G.V.; Berdonosov, S.S.; Murav' eva, I.A.; Martynenko, L.I. (Moskovskij Gosudarstvennyj Univ. (USSR))

1984-08-01

The static method and the flow method using /sup 91/Y and /sup 95/Zr radioactive indicators have been applied to determine pressure of saturated vapour of yttrium and zirconium acetylacetonates. Values of thermodynamic functions ..delta..Hsub(subl)=(98+-16)kJ/mol and ..delta..Ssub(subl.)=(155+-30)J/mol x K are calculated for sublimation of yttrium acetylacetonate. For sublimation of zirconium acetylacetonates ..delta..Hsub(subl) equals (116+-38) kJ/mol and ..delta..Ssub(subl) is equal to (198+-65) J/molxK.

Zirconium phosphate coating on aluminium foams by electrophoretic deposition for acidic catalysis

NARCIS (Netherlands)

Ordomskiy, V.; Schouten, J.C.; Schaaf, van der J.; Nijhuis, T.A.

2012-01-01

The electrophoretic deposition method has been applied for the formation of an amorphous zirconium phosphate layer on the surface of open-cell aluminum foam. The aluminum foam was fully and uniformly covered by the zirconium phosphate layer with a good mechanical adherence to the support. The

40 CFR 721.10152 - Oxirane, substituted silylmethyl-, hydrolysis products with alkanol zirconium(4+) salt and silica...

Science.gov (United States)

2010-07-01

...-, hydrolysis products with alkanol zirconium(4+) salt and silica, acetates (generic). 721.10152 Section 721... Oxirane, substituted silylmethyl-, hydrolysis products with alkanol zirconium(4+) salt and silica... zirconium(4+) salt and silica, acetates (PMN P-07-674) is subject to reporting under this section for the...

Reduced-Gravity Measurements of the Effect of Oxygen on Properties of Zirconium

Science.gov (United States)

Zhao, J.; Lee, J.; Wunderlich, R.; Fecht, H.-J.; Schneider, S.; SanSoucie, M.; Rogers, J.; Hyers, R.

2016-01-01

The influence of oxygen on the thermophysical properties of zirconium is being investigated using MSL-EML (Material Science Laboratory - Electromagnetic Levitator) on ISS (International Space Station) in collaboration with NASA, ESA (European Space Agency), and DLR (German Aerospace Center). Zirconium samples with different oxygen concentrations will be put into multiple melt cycles, during which the density, viscosity, surface tension, heat capacity, and electric conductivity will be measured at various undercooled temperatures. The facility check-up of MSL-EML and the first set of melting experiments have been successfully performed in 2015. The first zirconium sample will be tested near the end of 2015. As part of ground support activities, the thermophysical properties of zirconium and ZrO were measured using a ground-based electrostatic levitator located at the NASA Marshall Space Flight Center. The influence of oxygen on the measured surface tension was evaluated. The results of this research will serve as reference data for those measured in ISS.

Formation of zirconium dioxide layers on microelectrode of zirconium. Inhibition of the hydrogen evolution reaction

Czech Academy of Sciences Publication Activity Database

Pospíšil, Lubomír; Fanelli, N.; Hromadová, Magdaléna

2017-01-01

Roč. 49, C (2017), s. 128-133 ISSN 0324-1130 R&D Projects: GA ČR(CZ) GA16-03085S Institutional support: RVO:61388955 Keywords : zirconium * ZrO2 * corrosion Subject RIV: CG - Electrochemistry OBOR OECD: Electrochemistry (dry cells, batteries, fuel cells, corrosion metals, electrolysis) Impact factor: 0.238, year: 2016

Synthesis and characterization of a mesoporous hydrous zirconium oxide used for arsenic removal from drinking water

International Nuclear Information System (INIS)

Bortun, Anatoly; Bortun, Mila; Pardini, James; Khainakov, Sergei A.; Garcia, Jose R.

2010-01-01

Powder (20-50 μm) mesoporous hydrous zirconium oxide was prepared from a zirconium salt granular precursor. The effect of some process parameters on product morphology, porous structure and adsorption performance has been studied. The use of hydrous zirconium oxide for selective arsenic removal from drinking water is discussed.

Zircon Carburation Studies as Intermediate Stage in the Zirconium Fabrication

International Nuclear Information System (INIS)

Almagro Huertas, V.; Saenz de Tejada Gonzalez, L.; Lopez Rodriguez, M.

1963-01-01

Zirconium carbide and carbonitride mixtures were obtained by Kroll's method.Reaction products have been identified by micrography and X-ray diffraction analysis. The optimum graphite content in the initial charge for the carburation reaction has been studied. zirconium, silicon and carbon content in the final product has been controlled as a function of current in the furnace and reaction time.Further chlorination of the final product was performed successfully. (Author) 16 refs

Bayesian model selection validates a biokinetic model for zirconium processing in humans

Science.gov (United States)

2012-01-01

Background In radiation protection, biokinetic models for zirconium processing are of crucial importance in dose estimation and further risk analysis for humans exposed to this radioactive substance. They provide limiting values of detrimental effects and build the basis for applications in internal dosimetry, the prediction for radioactive zirconium retention in various organs as well as retrospective dosimetry. Multi-compartmental models are the tool of choice for simulating the processing of zirconium. Although easily interpretable, determining the exact compartment structure and interaction mechanisms is generally daunting. In the context of observing the dynamics of multiple compartments, Bayesian methods provide efficient tools for model inference and selection. Results We are the first to apply a Markov chain Monte Carlo approach to compute Bayes factors for the evaluation of two competing models for zirconium processing in the human body after ingestion. Based on in vivo measurements of human plasma and urine levels we were able to show that a recently published model is superior to the standard model of the International Commission on Radiological Protection. The Bayes factors were estimated by means of the numerically stable thermodynamic integration in combination with a recently developed copula-based Metropolis-Hastings sampler. Conclusions In contrast to the standard model the novel model predicts lower accretion of zirconium in bones. This results in lower levels of noxious doses for exposed individuals. Moreover, the Bayesian approach allows for retrospective dose assessment, including credible intervals for the initially ingested zirconium, in a significantly more reliable fashion than previously possible. All methods presented here are readily applicable to many modeling tasks in systems biology. PMID:22863152

Phase and morphology evolution of (Na1-xKxNbO3 powders related to calcinations and K2CO3 content

Directory of Open Access Journals (Sweden)

Steven J. Milne

2007-03-01