• Journal of Institute of Control, Robotics and Systems
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• v.19 no.10
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• pp.891-895
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• 2013

This paper proposes the development of a new method for online analysis which measured acid concentration in a pickling line. Pickling is the most important step to remove surface scale layers and is strongly depending on the exactly controlled pickling liquor composition. Today, there is no feasible system available for the online control of pickling lines. Within this paper, new methods for online analysis of pickling liquors have been tested and implemented into an overall pickling process control tool. This method measured simultaneously the hydrochloric acid and iron ion concentration in a solution of hydrochloric acid by measuring the ultrasonic speed, the solution temperature, and the electrical conductivity. Experimental results showed excellent precision and the measurement error was ${\pm}2g/l$ compared with the neutralization titration measurement.

• Korean Chemical Engineering Research
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• v.55 no.6
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• pp.785-790
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• 2017

To collect zinc, Fe and Zn in spent pickling solution were extracted by using TBP (tributyl phosphate), and Zn was recovered from extracted solution to zinc oxalate particles by oxalic acid solution. The reusability of TBP solvent was also tested. The distribution coefficient of Zn was not affected by the concentration of Fe in spent pickling solution, almost constant with the values of 7.12~9.31 when extracted by TBP solvent. It was found that the extraction capacity of TBP solvent for Zn is higher than that for Fe. The extraction efficiency of Zn was higher than 95%, while most of Fe was left in aqueous phase. After the recovery, the used TBP solvent could be repeatedly reused for the extraction of Zn up to eight times. XRD analysis showed that zinc oxalate ($ZnC_2O_4$ $2H_2O$) was formed from the reaction of Zn-TBP and oxalic acid. From the results of SEM analysis, the formation of zinc oxalate particle was strongly affected by the concentration of oxalic acid. In summary, Zn in spent pickling solution was successfully separated and recovered with TBP solvent and oxalic acid solution, respectively.

• Clean Technology
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• v.11 no.1
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• pp.21-28
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• 2005

Nitric acid free pickling solution was applied to solve the severe environmental problems attributed to nitric acid during pickling process of stainless steel product. In points of pickling capability and erosion of stainless steel base metal, a solution contains I% of hydrochloric acid and 2% of hydrofluoric acid and hydrogen peroxide was revealed as the best alternative to conventional mixed acid of nitric acid and hydrofluoric acid. To keep the pickling capability, it was necessary to maintain the concentration ratio of hydrogen peroxide to hydrochloric acid above 0.5.

• Resources Recycling
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• v.26 no.5
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• pp.97-104
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• 2017

Nuclear fuel cladding tubes are manufactured through pilgering and the annealing process. In order to remove the oxidized layer and impurities on the surface of the tube, a pickling process is required. Zirconium (Zr) is dissolved in a HF and $HNO_3$ acid mixture during the process and the pickling waste acid, including the dissolved Zr, is completely discarded after neutralization. This study observes the effects of the residual impurities (Ba) in the pickling solution regenerated from the $BaF_2$ precipitation process on the waste pickling solution. In addition, the concentration of Ba and Zr for the actual nuclear fuel cladding tube process was optimized. The regenerated pickling solution was tested through a pilot plant pickling process device that simulates the commercial pickling process of nuclear fuel cladding tubes, and the pickling efficiency was analyzed through AFM analysis of the roughness of the cladding tube surface.

• The Korean Journal of Food And Nutrition
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• v.12 no.1
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• pp.55-62
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• 1999

Changes in the alliinase activity during the aging of pickled garlic samples prepared by the several methods were investigated. The activity of alliinase in raw garlic was 8,37 units/mg protein. The ac-tivity in the garlic pickled with swoy sauce was reduced to 4.57 units/mg with 52% remaining by 1st week of pickling and to 1.05 units/mg protein with 12% remaining by 2nd week of pickling. The ac-tivity of alliinase in the garlic pickled with vinegar was 2.79 units/mg protein with 32% remaining by 1st week of pickling and was 0.26 units/mg protein only with 3% remaining by 2nd week of pickling. The activity of alliinase in the garlic pickled with 10% salt solution was 5.06 units/mg protein with 58% remaining by 1st week of pickling. After one week pickling the juice of pickled garlic was removed. Then garlics were pickled again with vinegar. The allinase acting in was reduced to 0.85 units/mg pro-tein with 10% remaining by 2nd week of pickling. The activity of alliinase in the garlic pickled with vin-egar was 2.79 units/mg protein with 32% remaining by 1st week of pickling. The juice of pickled garlic was removed after one week. Then the galics were again pickled with saysauce. The allinase activity in the garlic the garlic pickled again with soy sauce was reduced to 0.43 units/mg protein with 5% remain-ing by 2 week of pickling.

• Korean Journal of Materials Research
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• v.27 no.12
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• pp.672-678
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• 2017

In the production of zirconium cladding tube, a pickling acid solution is used to remove surface contaminants, which generates tons of pickling acid waste. The waste pickling solution is a valuable resource of Hf-free Zr. Many studies have investigated separating the Hf-free Zr source from the waste pickling acid. The results showed that $Ba_2ZrF_8$ precipitates prepared from the waste pickling acid were useful as an electrolyte for the electrorefining of Zr in molten salt. In the present work, electrorefining was performed in a $Ba_2ZrF_8-LiF$ binary electrolyte to recover Zr from a Hf-free CuZr ingot anode prepared by electroreduction. Before electrorefining, two pretreatments are performed. First, electrolyte melting was carried out to determine the eutectic temperature, and second, the electrolyte was treated to eliminate impurities, mainly hydride. After electrorefining, the cathode deposits were analyzed by $O_2$ gas analyzer and SEM-EDX to explore the possibility of recovering nuclear-grade Zr metal. Moreover, the anode was analyzed by SEM-EDX to determine the Zr dissolution depth.

• Journal of the Korean Ceramic Society
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• v.13 no.1
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• pp.25-29
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• 1976

The properties vary with quality of ferric-oxide that is major material of ferrites. In this point of view, a manufacturing method of pure and homogeneous fine ferric oxide is very important. The characters of this study are as follows: 1) Ferric oxide was made from waste pickling liquor of steel. 2) The crude ferric-oxide that is made by roasting the pickling liquor was dissolved in 20% HCI solution and then produced ferric chloride is purified by ethyl ether extraction. 3) The methanol solution of purified ferric chloride was sprayed into the refractory tube with compressed air and propane gas and then ignited leading to the ferric-oxide powder. 4) The produced oxide powder was introduced to the scrubber type vessel throught cooling system in order to collect the powder. 5) Crystalline phase of the powder was identified by X-ray diffraction and particle size, crystalline shape of the powder were investigated by settling method and electron microscope and the effects of concentration of ferric chloride in methanol on grain size were discussed. Results were obtained as fellows: 1) Total impurity in the ferric oxide produced from waste pickling liquor was 3.7%. 2) The solubilityof crude ferric oxide that was made from waste pickling liquor in HCI solution increased with the HCI concentration and reached to saturation range at 15% HCI concentration. 3) Extraction of FeCl3 increased with HCI concentration which is solvent. 4) Alpha ferric oxide obtained was very fine crystalline particles, the mean crystalline grain increased with the concentration of ferric chloride, and mean grain size distributed from 3.5$\mu$(at 0.5mole/l) to 0.5$\mu$(at 0.05mole/l).

• Resources Recycling
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• v.17 no.2
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• pp.36-45
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• 2008

Pickling of oxidized 304 stainless steel has been investigated using rotating disk electrode in waste acid solutions generated from the etching process of silicon wafer in order to recycle them. The waste acid solution contained acetic, nitric, hydrofluoric acids, and silicon of $19.6g/L^{-1}$. Electrochemical behavior during the pickling was distinctively different between the original and silicon-removed acid solutions. Open circuit potential was continuously changed in the original solution, while it was discontinuously changed and fluctuated in the silicon-removed solution. Fast and abrupt removal of surface oxide layer with severe pitting was observed in the silicon-removed solution. It was found that solution temperature had the most influential effect on glossiness. Surface glossiness after pickling was decreased with solution temperature. At the same condition, the glossiness was higher in the original solution than in the silicon-removed solution.

• Korean Journal of Materials Research
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• v.29 no.8
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• pp.483-490
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• 2019

Currently, the Korean nuclear industry uses ZIRLO as material for nuclear fuel cladding(zirconium alloy). KEPCO Nuclear Fuel is in the process of developing a HANA alloy to enable domestic production of cladding. Cladding manufacture involves multistage heat treatments and pickling processes, the latter of which is vital for the removal of defects and impurities on the cladding surface. SMUT that forms on the cladding surface during such pickling process is a source of surface defects during heat treatment and post-treatment processes if not removed. This study analyzes ZIRLO, HANA-4, and HANA-6 alloy claddings to extensively study the SEM/EDS, XRD, and particle size characteristics of SMUT, which are second phase particles that are formed on the cladding surface during pickling processes. Using the analysis results, this study observes SMUT formation characteristics according to Nb concentration in Zr alloys during the washing process following the pickling process. In addition, this study observes SMUT removal characteristics on cladding surfaces according to concentrations of nitric acid and hydrofluoric acid in the acid solution.

• Journal of the Korean institute of surface engineering
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• v.49 no.1
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• pp.62-68
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• 2016

A chromium-free Ce-based conversion coating formed by immersion in a solution containing cerium chloride and nitric acid on AZ31 magnesium alloy has been studied. The effects of acid pickling on the morphology and the corrosion resistance of the cerium conversion coating were investigated. The corrosion resistance of the conversion coating prepared on AZ31 Mg alloy after organic acid pickling was better than that of inorganic acid pickling. The morphology of the conversion-coated layer was observed using optical microscope and SEM. Results show that the conversion coatings are relatively uniform and continuous, with thickness 1.0 to $1.1{\mu}m$. The main elements of the conversion coating of AZ31 Mg alloy are Mg, O, Al, Ce and Zn by EDS analysis. The electrochemical polarization results showed that the Ce-based conversion coating could reduce the corrosion activity of the AZ31 Mg alloy substrates in the presence of chloride ions.