• 제어로봇시스템학회논문지
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• 제19권10호
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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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• 제55권6호
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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.

• 청정기술
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• 제11권1호
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• pp.21-28
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• 2005

스테인레스강의 산세공정에서 사용하는 질산으로 인한 환경문제를 해결하기 위하여 질산을 포함하지 않는 새로운 산세용액을 개발하고자 하였다. 산세용액의 반복 사용 시의 산세성능과 모재의 침식 정도를 기준으로 연구한 결과, 산 1%, 불산 및 과산화수소 각 2% 의 조성을 갖는 용액이 기존의 질산-불산 용액과 유사한 수준의 우수한 산세특성을 나타내었다. 또한 산세능을 유지하기 위해서는 염산 대비 과산화수소의 비율을 0.5 이상 유지해야 하는 것으로 나타났다.

• 자원리싸이클링
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• 제26권5호
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• pp.97-104
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• 2017

핵연료 피복관(지르코늄 합금)은 필거링, 세정, 산 세정 및 열처리공정을 거쳐 만든다. 튜브 표면의 산화층과 불순물을 제거하기 위하여 산 세정(酸 洗淨, Acid pickling) 공정이 요구된다. 이때 산세 공정 중 불산과 질산의 혼합 산(酸) 용액으로부터 용해된 Zr이 농축된 폐산은 중화반응을 거쳐 전량 폐기 처리 된다. 본 연구에서는 $BaF_2$ 침전 공정을 통해 재생산된 산세 용액의 잔존 불순물(Ba)이 산세에 미치는 영향을 관찰하였다. 이와 더불어 실제 핵연료 피복관의 산세 공정에 적합한 재생산 제조를 위한 잔존 Ba 및 Zr의 농도 저감 실험을 실시하여 최적 침전 공정 조건을 도출하였으며, 핵연료 피복관의 산세 공정을 모사한 파일럿 플랜트 산세공정 장치에서 재생산된 산세용액을 사용하여 피복관의 산세 효율을 AFM 분석을 통해 관찰하였다.

• 한국식품영양학회지
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• 제12권1호
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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.

• 한국재료학회지
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• 제27권12호
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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.

• 한국세라믹학회지
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• 제13권1호
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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).

• 자원리싸이클링
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• 제17권2호
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• pp.36-45
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• 2008

실리콘 웨이퍼 에칭공정에서 발생하는 폐산을 스테인리스 스틸 산세공정에서 재활용하고자 이를 이용한 산세 거동을 조사하였다. 폐산 원액은 $19.6g/L^{-1}$ 실리콘을 함유한 불산, 질산 및 초산의 혼산이었으며 침전법에 의한 실리콘 제거 전후 폐산들을 이용하여 304 스테인레스 스틸 표면 산화막의 제거 시 측정된 open circuit potential(OCP) 변화 거동은 매우 상이하였다. 폐산 원액을 사용한 경우에는 OCP가 높고 연속적인 변화를 보이는데 비하여 실리콘 제거 공정에서 얻어진 용액의 경우에는 불연속적인 OCP변화와 전위요동현상이 나타났다. 이러한 거동의 차이는 표면 부동태막의 형성 및 제거와 공식이 발생하는 정도의 차이에 기인하는 것으로 생각되며, 실리콘 제거 공정에서 산도가 낮아진 폐산에서 산화막 제거속도가 높고 공식발생이 현저하였다. 산세 후 시료의 표면 광택도에 가장 큰 영향을 주는 것은 산세 온도였으며, 산세온도가 높아질수록 표면 광택도는 감소하였다. 동일 산세 조건에서는 폐산 원액을 사용한 경우가 실리콘을 제거공정으로부터 얻어진 용액을 사용한 경우보다 광택도가 높았다.

• 한국재료학회지
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• 제29권8호
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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.

• 한국표면공학회지
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• 제49권1호
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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.