• Journal of Conservation Science
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• v.25 no.4
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• pp.399-409
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• 2009

Outdoor iron artefacts are easily corroded by affection of environmental pollutants directly. Especially they need to be removed $Cl^-$ ions, but outdoor iron artefacts are excluded for desalination owing to their special features. Therefore this study contains the conservation processes of an iron stele of the Joseon Dynasty as the sample as well as desalination experiments that were carried out the desalting method using spill pads and the immersion desalting method together in order to compare. Desalting methods were compared by analyses such as an optical and metallurgical microscope, SEM-EDS, pH meter, Ion Chromatography and X-ray diffraction. As a result of the analysis, the optical and metallurgical microscopy show that the corrosion products are constituted by the layers and the metallurgical microstructure is a white cast iron. The SEM-EDS results of corrosion products detected mainly Fe, O, and especially Cl upto 2.48wt%. The results of pH and anion analysis for the washing solution, the desalting method using spill pads shows the similar effect to the immersion desalting method. As a result of XRD analysis before and after desalting corrosion products, goethite, magnetite, lepidocrocite and akaganeite are detected before desalting, but akaganeite is not detected after desalting at the desalting methode using spill pads, which indicates to have an effect on desalination. Therefore the results show that the desalting method using spill pads has an effect on desalination similar to the immersing desalting method.

• Journal of the Korean institute of surface engineering
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• v.40 no.1
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• pp.44-56
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• 2007

Excavated archaeological iron artifacts are usually conducted the conservation treatment for removal of chloride ions in the corrosion products. However, some iron artifacts are corroded again even after the conservation treatment due to unremoved chloride ions. Therefore, it is important to prevent desalinized artifacts from the occurrence of corrosion after the treatment. In this paper, we investigated the characteristics of corrosion products on salinized iron artifacts and evaluated the variety of desalination methods such as autoclave, intensive washing and NaOH. It was also found that ${\beta}-FeOOH$ (Akaganeite) played an important role on the occurrence of corrosion and the treatment for removal of chloride ions. The extents of desalination were compared between the desalination methods. Results showed that the autoclave method represented the highest efficiency for desalination while the intensive washing method was the lowest.

• Journal of Powder Materials
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• v.15 no.2
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• pp.148-155
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• 2008

Nano magnetite particles have been prepared by two step reaction consisting of urea hydrolysis and ammonia addition at certain ranges of pH. Three different concentrations of aqueous solution of ferric ($Fe^{3+}$) and ferrous ($Fe^{2+}$) chloride (0.3 M-0.6 M, and 0.9 M) were mixed with 4 M urea solution and heated to induce the urea hydrolysis. Upon reaching at a certain pre-determined pH (around 4.7), 1 M ammonia solution were poured into the heated reaction vessels. In order to understand the relationship between the concentration of the starting solution and the final size of magnetite, in-situ pH measurements and quenching experiments were simultaneous conducted. The changes in the concentration of starting solution resulted in the difference of the threshold time for pH uprise, from I hour to 3 hours, during which the akaganeite (${\beta}$-FeOOH) particles nucleated and grew. Through the quenching experiment, it was confirmed that controlling the size of ${\beta}$-FeOOH and the attaining a proper driving force for the reaction of ${\beta}$-FeOOH and $Fe^{2+}$ ion to give $Fe_3O_4$ are important process variables for the synthesis of uniform magnetite nanoparticles.

• Journal of Microbiology and Biotechnology
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• v.18 no.9
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• pp.1572-1577
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• 2008

A facultative dissimilatory metal-reducing bacterium, Shewanella sp. strain HN-41, was used to produce magnetite nanoparticles from a precursor, poorly crystalline iron-oxyhydroxide akaganeite ($\beta$-FeOOH), by reducing Fe(III). The diameter of the biogenic magnetite nanoparticles ranged from 26 nm to 38 nm, characterized by dynamic light scattering spectrophotometry. The magnetite nanoparticles consisted of mostly uniformly shaped spheres, which were identified by electron microscopy. The magnetometry revealed the superparamagnetic property of the magnetic nanoparticles. The atomic structure of the biogenic magnetite, which was determined by extended X-ray absorption fine structure spectroscopic analysis, showed similar atomic structural parameters, such as atomic distances and coordinations, to typical magnetite mineral.

• Economic and Environmental Geology
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• v.47 no.4
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• pp.431-439
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• 2014

The purposes of this research were to investigate the enrichment of metal-reducing bacteria from KURT groundwater and the identification of the microbial diversity by 16S rRNA as well as to examine microbial Fe(III)/Mn(IV) reduction and to analyze morphological features of interactions between microbes and precipitates and their mineralogical composition. To cultivate metal-reducing bacteria from groundwater sampled at the KURT in S. Korea, different electron donors such as glucose, acetate, lactate, formate, pyruvate and Fe(III)-citrate as an electron accepter were added into growth media. The enriched culture was identified by 16S rRNA gene sequence analysis for the diversity of microbial species. The effect of electron donors (i.e., glucose, acetate, lactate, formate, pyruvate) and electron acceptors (i.e., akaganeite, manganese oxide) on microbial iron/manganese reduction and biomineralization were examined using the 1st enriched culture, respectively. SEM, EDX, and XRD analyses were used to determine morphological features, chemical composition of microbes and mineralogical characteristics of the iron and manganese minerals. Based on 16S rRNA gene analysis, the four species, Fusibacter, Desulfuromonas, Actinobacteria, Pseudomonas sp., from KURT groundwater were identified as anaerobic metal reducers and these microbes precipitated metals outside of cells in common. XRD and EDX analyses showed that Fe(III)-containing mineral, akaganeite (${\beta}$-FeOOH), reduced into Fe(II)/Fe(III)-containing magnetite ($Fe_3O_4$) and Mn(IV)-containing manganese oxide (${\lambda}-MnO_2$) into Mn(II)-containing rhodochrosite ($MnCO_3$) by the microbes. These results implicate that microbial metabolism and respiratory activities under anaerobic condition result in reduction and biomineralization of iron and manganese minerals. Therefore, the microbes cultivated from groundwater in KURT might play a major role to reduce various metals from highly toxic, mobile to less toxic, immobile.

• Journal of Conservation Science
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• v.29 no.4
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• pp.297-309
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• 2013

Iron objects become corroded at fast speed from the moment when they are excavated, so it is needed to control corrosion through processes of conservation treatment. However, re-corrosion mostly takes place in excavate iron objects, although they have already gone through the process of conservation treatment, and it is more difficult to carry out the second conservation treatment of re-corroded excavated iron objects than the first conservation treatment, and it requires a longer period of time to treat them as well. In this study, aims to discover factors of re-corrosion by scientifically analyzing corrosion products generated during the process of storage after the process of conservation treatment. The finished on conservation treatment of the iron artifacts, which were unearthed from three ancient site in Gyeongju by using the same conservation method between 2002 and 2009, re-corrosion condition observed on the packaging-iron artifacts. Focused on 9 target forged iron artifacts among them, this study analyzed the physical changes by mass measurement, naked-eye and microscopic observations and the chemical changes by SEM-EDS, XRD, IC and ICP analysis. The results show that the yellowish brown corrosion products formed on the facing surface of part dropped from the artifacts had different associated forms but acicular shape. In addition, the acicular shape became clearer as the color changed from red to yellowish brown. According to the process when the conservation treatment was completed, the mass of the artifacts increased in proportion to the corrosion products and the chloride ion ($Cl^-$) concentration had a tendency to increase relatively. ${\beta}$-FeOOH (akaganeite) was confirmed in the XRD analysis for the corrosion products of all the collected samples. As a result of ICP analysis, $Na^+$ and $Ca^{2+}$ components were confirmed.

• Journal of the Mineralogical Society of Korea
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• v.20 no.1 s.51
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• pp.47-60
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• 2007

While sedimentological researches on Western coastal tidal flats of Korea have been much pelformed previously, mineralogical and biogeochemical studies are beginning to be studied. The objectives of this study were to investigate mineralogical characteritics of the inter-tidal flat sediments and to explore phase transformation of iron(oxyhydr)oxides and biomineralization by metal-reducing bacteria enriched from the inter-tidal flat sediments from Muan, Jeollanam-do, Korea. Inter-tidal flat sediment samples were collected in Chungkye-myun and Haeje-myun, Muan-gun, Jeollanam-do. Particle size analyses were performed using the pipette method and sedimentation method. The separates including sand, silt and clay fractions were examined by scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM), and X-ray diffiaction (XRD). After enriching the metal-.educing bacteria from the into,-tidal flat sediments, the bacteria were used to study phase transformation of the synthesized iron (oxyhydr)oxides and iron biomineralization using lactate or glucose as the electron donors and Fe(III)-containing iron oxides as the electron accepters. Mineralogical studies showed that the sediments of tidal flats in Chung]rye-myun and Haeje-myun consist of quartz, plagioclase, microcline, biotite, kaolinite and illite. Biogeochemical researches showed that the metal-reducing bacteria enriched from the inter-tidal flat sediments reduced reddish brown akaganeite and mineralized nanometer-sized black magnetite. The bacteria also reduced the reddish brown ferrihydrite into black amorphous phases and reduced the yellowish goethite into greenish with formation of nm-sized phases. These results indicate that microbial Fe(III) reduction may play one of important roles in iron and carbon biogeochemistry as well as iron biomineralization in subsurface environments.

• Corrosion Science and Technology
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• v.17 no.2
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• pp.60-67
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• 2018

The compounds associated with corrosion, in metallic archaeological samples of carbon steel of insular origin were evaluated to establish their degree of deterioration and structural damage against air pollution. The iron phases present in samples of archaeological artifacts were detected by Raman spectroscopy and confocal Raman microcopy. These samples mainly exhibited ing mainly ${\beta}$-FeO(OH) type goethite oxyhydroxides and small amounts of akaganeite ${\alpha}$-FeO(OH) lepidocrocite ${\gamma}$-FeO(OH) due to dominant chloride in a marine environment and non-stoichiometric oxyhydroxides Fe (II + / III +) as indicators of early corrosion. Some parts showed the presence of magnetic maghemite indicating high corrosion. ${\gamma}$-FeO(OH) is a precursor of phases associated with advanced marine corrosion. By studying its decomposition by Raman spectroscopy, it was synthesized with the following sequence: ${\gamma}-FeO(OH){\rightarrow}{\alpha}-FeO(OH)+{\gamma}-FeO(OH)$, ${\rightarrow}{\gamma}-Fe_2O_3+Fe_3O_4$. Ferric compounds provided evidence for the effect of intensity of laser on them, constituting a very useful input for the characterization of oxidation of iron in this type of artifacts. Thus, destructive analysis techniques should be avoided in addition to the use of small amounts of specimen.

• Journal of the Mineralogical Society of Korea
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• v.16 no.1
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• pp.107-123
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• 2003

The objective of this study was to investigate mineral precipitates, which derived from the zero valent iron (ZVI) corrosion during TCE dechlorination and to find the controlling factors in mineral precipitates. A series of column experiemnts were conducted to evaluate the location of ZVI and the effects of electrode arrangements in electro-enhanced permeable reactive barrier (E2PRB) systems. Based on mineralogical study, ZVI samples near the influent port had more lepidocrocite, ferrihydrite or Fe (oxy)hydroxide, and (phospho)siderite while backward samples had more akaganeite, magnetite/maghemite, and intermediate green rust (GR) I and GR II. A suite of mineral distribution was preferabley related to the dissolved oxygen and the increased pH. Controlling factors of mineral precipitates in an E2PRB system were found to be (1) pH, (2) dissolved oxygen, (3) the types of Fe intermediates, and (4) anionic species to form complex strongly.

• Journal of Soil and Groundwater Environment
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• v.11 no.6
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• pp.35-42
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• 2006

Experimental study was conducted to identify the active agent for reductive dechlorination of TCE in cement/Fe(II) systems. Several potential materials-hematite (${\alpha}-Fe_2O_3$), lepidocrocite (${\gamma}$-FeOOH), akaganeite (${\beta}$-FeOOH), ettringite ($Ca_6Al_2(SO_4)_3(OH)_{12}$)-that are cement components or parts of cement hydrates were tested if they could act as reducing agents by conducting TCE degradation experiments. From the initial degradation experiments, hematite was selected as a potential active agent. The pseudo-first-order degradation rate constant ($k\;=\;0.637\;day^{-1}$) for the system containing 200 mM Fe(II), hematite and CaO was close to that ($k\;=\;0.645\;day^{-1}$) obtained from the system containing cement and 200 mM Fe(II). CaO, which was originally added to simulate pH of the cement/Fe(II) system, was found to play an important role in degradation reactions. The reactivity of the hematite/CaO/Fe(II) system initially increased with increase of CaO dosage. However, the tendency declined in the higher CaO dosage region, implying a saturation type of behavior. The SEM analysis revealed that the hexagonal plane-shaped crystals were formed during the reaction with increasing degradation efficiency, which was brought about by increasing the CaO dosage. It was suspected that the crystals could be portlandite or green rust ($SO_4$) or Friedel's salt. The XRD analysis of the same sample identified the peaks of hematite, magnetite/maghemite, green rust ($SO_4$). Either instrumental analysis predicted the presence of the green rust ($SO_4$). Therefore, the green rust ($SO_4$) would potentially be a reactive agent for reductive dechlorination in cement/Fe(II) systems.