• Analytical Science and Technology
• /
• v.23 no.1
• /
• pp.45-53
• /
• 2010

For the determination of chlorine in uranium compound, analytical methods by using a steam distillation and a pyrohydrolysis have been developed. The steam distillation apparatus was composed of steam generator, distilling flask and condenser etc. The samples were prepared with an aliquot of LiCl standard solution and a simulated spent nuclear fuel. A sample aliquot was mixed with a solution containing 0.2 M ferrous ammonium sulfate-0.5 M sulfamic acid 3 mL, phosphoric acid 6 mL and sulfuric acid 15 mL. The chloride was then distilled by steam at the temperature of $140^{\circ}C$ until a volume of $90{\pm}5\;mL$ is collected. The pyrohydrolysis equipment was composed of air introduction system, water supply, quartz reaction tube, combustion tube furnace, combustion boat and absorption vessel. The chloride was separated from powdered sample which is added with $U_3O_8$ accelerator, by pyrohydrolysis at the temperature of $950^{\circ}C$ for 1 hour in a quartz tube with a stream of air of 1 mL/min supplied from the water reservoir at $80^{\circ}C$. The chlorides collected in each absorption solution by two methods was diluted to 100 mL and measured with ion chromatography to determine the recovery yield. For the ion chromatographic determination of chlorine in molten salt retained in a metal ingot, the chlorine was separated by means of pyrohydrolysis after air and dry oxidation, and grinding for the sample.

• Resources Recycling
• /
• v.32 no.1
• /
• pp.21-32
• /
• 2023

Because the application of lithium has gradually increased for the production of lithium ion batteries (LIBs), more research studies about recycling using solvent extraction (SX) should focus on Li⁺ recovery from the waste solution obtained after the removal of the valuable metals nickel, cobalt and manganese (NCM). The raffinate obtained after the removal of NCM metal contains lithium ions and other impurities such as Na ions. In this study, we optimized a selective SX system using di-(2-ethylhexyl) phosphoric acid (D2EHPA) as the extractant and tri-n-butyl phosphate (TBP) as a modifier in kerosene for the recovery of lithium from a waste solution containing lithium and a high concentration of sodium (Li⁺ = 0.5 ~ 1 wt%, Na⁺ = 3 ~6.5 wt%). The extraction of lithium was tested in different solvent compositions and the most effective extraction occurred in the solution composed of 20% D2EHPA + 20% TBP + and 60% kerosene. In this SX system with added NaOH for saponification, more than 95% lithium was selectively extracted in four extraction steps using an organic to aqueous ratio of 5:1 and an equilibrium pH of 4 ~ 4.5. Additionally, most of the Na⁺ (92% by weight) remained in the raffinate. The extracted lithium is stripped using 8 wt% HCl to yield pure lithium chloride with negligible Na content. The lithium chloride is subsequently treated with high purity ammonium bicarbonate to afford lithium carbonate powder. Finally the lithium carbonate is washed with an adequate amount of water to remove trace amounts of sodium resulting in highly pure lithium carbonate powder (purity > 99.2%).

• Bulletin of the Korean Chemical Society
• /
• v.33 no.5
• /
• pp.1669-1674
• /
• 2012

A novel superabsorbent composite was prepared by intercalation polymerization of acrylic acid (AA) and 2-acrylamido-2-methyl-1-propane sulfonic acid (AMPS) in the presence of montmorillonite (MMT), using ammonium persulfate (APS) as an initiator and $N,N'$-methylenebisacrylamide (MBA) as a cross linker. The superabsorbent composite was characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), X-ray diffraction (XRD) and thermogravimetric analysis (TGA). Maximum absorbency of the composite in distilled water and 0.9% sodium chloride solution was 722 and 108 g/g, respectively. The composite was used for removal of heavy metal ions from aqueous solutions. Maximum amount of adsorption for $Ni^{2+}$, $Cu^{2+}$ and $Pb^{2+}$ was 211.0, 159.6 and 1646.0 mg/g, respectively, and the adsorption was in accordance with both Langmuir and Freundlich model. The composite could be regenerated and reused in wastewater treatment.

• Journal of the Korean institute of surface engineering
• /
• v.48 no.2
• /
• pp.68-72
• /
• 2015

The corrosion behavior of metals and alloys for the safety of offshore structures in seawater was investigated for the application of sacrificial anodes. The experiments were focused on the polarization behaviors and the surface morphology of each metal after experiments. Pure Zn, pure Al (Al1050), Al alloys (Al5052, Al6061), Mg alloys (AZ31, AZ91D) and steel (SCM440) were assessed in 3.5% sodium chloride solution by means of potentiodynamic polarization to verify the galvanic corrosion potential ($E_{couple}$). Potentiostat plots were plotted to compare the surface and corrosion current density ($i_{couple}$) of metals as sacrificial anodes in seawater to protect steel alloy as a cathode. Al alloys showed the best performance as a sacrificial anode, on the other hand, Mg alloys showed overprotection behavior. The surface morphologies of sacrificial anodes were observed by FESEM and compared.

• Journal of the Korean Chemical Society
• /
• v.43 no.1
• /
• pp.36-41
• /
• 1999

The adsorptive stripping voltammetric determination method of trace germanium (IV) using mercaptoacetic acid as a ligand was studied. Optimal conditions were found to be 0.25 M NaCl solution (pH 6.0) containing mercaptoacetic acid concentration of $5.0{\times}10^{-6}M$. The peak potential appeared at - 1.402 V vs. Ag/AgCl. Effects of sodium chloride concentration, mercaptoacetic acid concentration, and accumulation time for the complex of Ge(IV)-Mercaptoacetic acid on the peak current were studied. Amberlite IRC-718 chelating resin was applied to the separation of Ge(IV) from other metal ions.

• Journal of Powder Materials
• /
• v.11 no.4
• /
• pp.322-327
• /
• 2004

Ultrafine titanium carbide particles were synthesized by the reaction of liquid-magnesium and vaporized TiCl$_{4}$+C$_{x}$Cl$_{4}$(x = 1 and 2) solution. Fine titanium carbide particles with about 50 nm were successfully produced by combining Ti and C atoms released by chloride reduction of magnesium, and vacuum was then used to remove the residual phases of MgCl$_{2}$ and excess Mg. Small amounts of impurities such as O, Fe, Mg and Cl were detected in the product, but such problem can be solved by more precise process control. The lattice parameter of the product was 0.43267 nm, near the standard value. With respect to the reaction kinetics, the activation energy for the reactions of TiCl$_{4}$+C$_{2}$Cl$_{4}$and Mg was found to 69 kJ/mole, which was about half value against the use of TiCl$_{4}$+CCl$_{4}$, and such higher reactivity of the former contributed to increase the stoichiometry until the level of TiC$_{0.96}$ and decrease the free carbon content below 0.3 wt.%.

• Bulletin of the Korean Chemical Society
• /
• v.26 no.1
• /
• pp.38-42
• /
• 2005

Bis(2-methylbenzaldehyde)butane-2,3-dihydrazone(TDSB) was used as new N-N Schiff's base which plays the role of an excellent ion carrier in the construction of a La(III) membrane sensor. The best performance was obtained with a membrane containing, 30% poly(vinyl chloride), 60% benzyl acetate, 6% TDSB and 4% sodium tetraphenyl borate. This sensor reveals a very good selectivity towards La(III) ions over a wide variety of cations, including alkali, alkaline earth, transition and heavy metal ions. The proposed electrode exhibits a Nernstian behavior (with slope of 19.8 mV per decade) over a wide concentration range (1.0 ${\times}$ 10$^{-5}$-1.0 ${\times}$ 10$^{-1}$ M). The detection limit of the sensor is 7.0 ${\times}$ 10$^{-6}$ M. It has a very short response time, in the whole concentration range ($\sim$5 s), and can be used for at least twelve weeks in the pH range of 3.0-9.4. The proposed sensor was successfully applied as an indicator electrode for the potentiometric titration of a La(III) solution, with EDTA. It was also successfully applied in the determination of fluoride ions in three mouth wash preparations.

• Journal of environmental and Sanitary engineering
• /
• v.17 no.1
• /
• pp.63-68
• /
• 2002

Amount of styrene and divinylbenzene(DVB) was adjusted under injection of nitrogen, copolymer having crosslink of 1%, 2% and 5% was synthesized and zinc chloride was added to it. Put into benzene, swell it, add potassium iodide and 1-aza-15-crown-5 of 21.93g in toluene solution and functional resin which can adsorb heavy metal ions by stir reflex at $55^{\circ}C$ for 30 hours was synthesized. The content of divinylbenzene of this resin was increased as crosslink increase, macroporous gets smaller and the content of chlorine was reduced, which affects macrocyclic ligand in the process of substitution and content of nitrogen was also reduced. And the form of functional synthetic resin was distorted by substitution reaction of hydrogen and chlorine atoms.

• Journal of the Korean institute of surface engineering
• /
• v.40 no.2
• /
• pp.82-90
• /
• 2007

Crevice corrosion is the accelerated attack occurred in the occluded cell under a crevice on the metal surface. Crevice corrosion behaviors of nickel-based alloys such as Alloy 600 and Alloy 690 were investigated in acidic solution with different chloride ion concentrations. Tests were carried out using the specially designed crevice cell with a very narrow Luggin capillary assembly to measure the potential inside the crevice. It is believed that crevice corrosion in active/passive system like nickel-based alloys has much to do with the properties of passive film and its repassivation characteristics, investigated by the capacitance measurement and by the abrading electrode technique, respectively. An attempt was made to elucidate the relationship between crevice corrosion behaviors, properties of passive film and its repassivation kinetics. Results showed that repassivation rate parameter $n1{\leq}0.6$ and/or $n2{\leq}0.5$ indicated the possible occurrence of crevice corrosion.

• Journal of Welding and Joining
• /
• v.32 no.4
• /
• pp.26-33
• /
• 2014

The metallurgical and mechanical characteristics, toughness and corrosion resistance of dissimilar welds between super duplex stainless steel UNS S32750 and carbon steel ASTM A516Gr.70 have been evaluated. Three heat inputs of 21.12, 24.00, 26.88kJ/cm were employed to make joints of dissimilar metals with flux cored arc welding(FCAW). Based on microstructural examination, vermicular ferrite was formed in the first layer of weld at low heat input(21.12kJ/cm) and $Cr_{eq}/Ni_{eq}$ of 1.61 while acicular ferrite was formed in last layer of weld at high heat input(26.88kJ/cm) and $Cr_{eq}/Ni_{eq}$ of 1.72. Ferrite percentage in dissimilar welds was lowest in the first layer of weld regardless of heat inputs and it gradually increased in the second and third layers of weld. Heat affected zone showed higher hardness than the weld metal although reheated zone showed lower hardness than weld metal due to the formation of secondary austenite. Tensile strengths of dissimilar welds increased with heat input and there was 100MPa difference. The corrosion test by ferric chloride solution showed that carbon steel had poor corrosion resistance and pitting corrosion occurred in the first layer(root pass) of weld due to the presence of reheated zone where secondary austenite was formed. The salt spray test of carbon steel showed that the surface only corroded but the amount of weight loss was extremely low.