• 제목/요약/키워드: 염화물 추출법

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Evaluation of Chloride Extraction under Electrochemical Chloride Extraction (전기화학적 염화물 추출법에 따른 염소이온 제거 성능 평가)

  • Jiseok, Kim;Ki-Yong, Ann
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.10 no.4
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    • pp.553-557
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    • 2022
  • The present study evaluate the chloride extracion under electrochemical chloride extraction method. Chloride was penetrated into the concrete from external reservoir using a 4M NaCl solution, and an electrochemical chloride extraction method was applied after the curing period of 1 year. The current density was constantly kept 1000 mA/m2 for coulostatic application with the variation in potential difference. The duration of the ECE treatment was 2, 4, 8 weeks, respectively. The residual chloride concentration at all depths decreased, and the chloride concentration decreased as the application period increased. After the application period of 8 weeks, 62.9 to 77.6 % of chloride extracted in the total chloride profile, and 77.7 to 99.5 % of chloride extracted in the free chloride profile. In particular, the concentration of free chloride at a depth of 7 mm or more from the concrete surface was 0.01 % or less by cement. In addition, it was confirmed that the bound chloride could be extracted by the electrochemical chloride extraction.

A study of semi-quantification of the Friedel's salt using the X-ray diffraction method in concrete (콘크리트 내 Friedel염의 XRD를 이용한 반정량적 측정기법에 관한 연구)

  • Lee, Ho-Jae;Lee, Jang-Hwa;Kim, Do-Gyeum
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.33-38
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    • 2012
  • Despite the importance of chloride binding, it is very difficult to measure the binding capacity, in particular, for the concrete body in an existing structure: in fact, the measurement procedure for chloride binding is much influenced by the environmental condition such as temperature, fineness of sample and pore water extraction techniques. The present study concerns the quantification of the binding capacity of chloride ions in concrete using the X-ray diffraction (XRD) technique. Once the binding isotherm of chlorides was determined by the Langmuir isotherm, as a function of the W/C, curing age and binder type, the generation of bound chlorides (i.e. Friedel's salt) was simultaneously ensured by the XRD technique. The amount of bound chloride was then determined by analyzing the peak intensity for the bound chlorides in the XRD curve. It was found that an increase in the curing age and a decrease in the W/C resulted in an increase in the binding capacity.

Recovery of Nickel from Waste Iron-Nickel Alloy Etchant and Fabrication of Nickel Powder (에칭 폐액으로부터 용매추출과 가수분해를 이용한 니켈분말제조에 관한 연구)

  • Lee, Seokhwan;Chae, Byungman;Lee, Sangwoo;Lee, Seunghwan
    • Clean Technology
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    • v.25 no.1
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    • pp.14-18
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    • 2019
  • In general after the etching process, waste etching solution contains metals. (ex. Nickel (Ni), Chromium (Cr), Zinc (Zn), etc.) In this work, we proposed a recycling process for waste etching solution and refining from waste liquid contained nickel to make nickel metal nano powder. At first, the neutralization agent was experimentally selected through the hydrolysis of impurities such as iron by adjusting the pH. We selected sodium hydroxide solution as a neutralizing agent, and removed impurities such as iron by pH = 4. And then, metal ions (ex. Manganese (Mn) and Zinc (Zn), etc.) remain as impurities were refined by D2EHPA (Di-(2-ethylhexyl) phosphoric acid). The nickel powders were synthesized by liquid phase reduction method with hydrazine ($N_2H_4$) and sodium hydroxide (NaOH). The resulting nickel chloride solution and nickel metal powder has high purity ( > 99%). The purity of nickel chloride solution and nickel nano powders were measured by EDTA (ethylenediaminetetraacetic) titration method with ICP-OES (inductively coupled plasma optical emission spectrometer). FE-SEM (field emission scanning electron microscopy) was used to investigate the morphology, particle size and crystal structure of the nickel metal nano powder. The structural properties of the nickel nano powder were characterized by XRD (X-ray diffraction) and TEM (transmission electron microscopy).

Overview on the Technologies for Extraction of Rare Earth Metals (희토류금속(稀土類金屬) 제련기술(製鍊技術) 개요)

  • Park, Hyung-Kyu;Lee, Jin-Young;Cho, Sung-Wook;Kim, Joon-Soo
    • Resources Recycling
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    • v.21 no.3
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    • pp.74-83
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    • 2012
  • Rare earth metals have been made from rare earth compounds which were prepared from rare earth ore concentrates through successive processes such as leaching(i.e. extraction of rare earth elements to liquid media), separation, purification, precipitation. Here, process for treating monazite and bastnasite ore concentrates were briefly reviewed, and metallothermic reduction and fused salt electrolysis methods were introduced as the extraction technologies for rare earth metals.

Competitive Extraction of Chlorinated Solvents by Headspace SPME GC/FID (Headspace SPME GC/FID를 이용한 Chlorinated Solvents의 경쟁적 추출효과에 관한 연구)

  • An, Sangwoo;Kim, Youngju;Chun, Sukyoung;Lee, Sijin;Park, Jaewoo;Chang, Soonwoong
    • Journal of the Korean GEO-environmental Society
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    • v.11 no.5
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    • pp.61-67
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    • 2010
  • In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of chlorinated solvents (PCE and TCE) and these by-products (cis-DCE, VC, and Ethylene). Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of chlorinated solvents and these by-products. The general affinity of analytes to CAR/PDMS fiber was high in the order PCE>TCE>cis-DCE>VC>Ethylene. The linearity of $R^2$ for chlorinated solvents and these by-products was from 0.912 to 0.999 when analyte concentrations range from $10{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.1% to 3.6% for concentration of $500{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for chlorinated solvents and these by-products were from $0.5{\mu}g/L$ to $10{\mu}g/L$, respectively.

Comparison of Colorimetric Methods for the Determination of Flavonoid in Propolis Extract Products (프로폴리스추출물 제품의 플라보노이드 함량분석을 위한 비색법의 비교)

  • Kim, Eun-Jeong;Lee, Hwa-Jung;Kim, Hye-Jeong;Nam, Hye-Seon;Lee, Mi-Keong;Kim, Hae-Young;Lee, Jin-Ha;Kang, Yun-Sook;Lee, Jong-Ok;Kim, Hee-Yun
    • Korean Journal of Food Science and Technology
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    • v.37 no.6
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    • pp.918-921
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    • 2005
  • Quantitative analysis of flavonoids in commercial propolis extract products were compared by three colorimetric methods; aluminum chloride method, dinitrophenylhydrazine method and aluminum nitrate method, Aluminum nitrate method in Korea Health Supplement Food Code was proved to be specific only for flavones and flavonols same as aluminum chloride method, while dinitrophenylhydrazine method was specific for flavanones and dihydroflavonols. Therefore, the sum of flavonoid contents determined by 2,4-Dinitrophenylhydrazine method and aluminum nitrate method may represent the real content of total flavonoids. As for the 25 commercial propolis extract products examined, the contents of flavonoid varied from 2.15% to 9.53% except for one product.

Differentiation of Sorptive Bindings of Some Radionuclides with Sequential Chemical Extractions in Sandstones (순차적화학추출법을 사용한 방사성핵종의 사암에 대한 수착유형 평가)

  • Park, Chung-Kyun;Hahn, Pil-Soo;Park, Hun-Hwee
    • Nuclear Engineering and Technology
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    • v.26 no.4
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    • pp.461-470
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    • 1994
  • Sorption experiments of $^{60}$ Co, $^{85}$ Sr. and $^{137}$ Cs onto sandstone particles in a batch were carried out to investigate the migration mobility. Sorption kinetics and reversibility as well as sorption mechanisms were examined. Sorption reaction occurred mostly within 10 hours on the outer surface of the sandstone particle but diffusion into the inner surface of the mineral has still occurred after that time. In order to distinguish sorption types of radionuclides, a sequential chemical extraction was introduced. The sorbed radionuclides were then extracted by applying different solutions of synthetic groundwater, CaCl$_2$, KCl and KOX-HA Especially KCl is adopted to extract the ion-exchanged cesium. Sorption types considered are reversible sorption under groundwater condition, ion exchange, association with ferro-manganese oxides or oxyhydroxides, and irreversible fixation. Strontium sorbs onto the sandstone surface mainly by fast and reversible ion exchange reaction. However, cobalt and cesium do not sorb by simple process. The main sorptive binding of cobalt was the association with ferro-manganese oxides and the secondary one was irreversible fixation. Diffusion into the lattice of minerals controlled the sorption rate of cobalt The main sorptin type of cesium was irreversible fixation, while ion exchange reaction was the secondary importance. Hence the oreder of migration mobility for the three radionuclides was Sr$^{2+}$ > Co$^{2+}$ > Cs$^{+}$ in the sandstones.

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Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.227-234
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    • 2019
  • An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

Synthesis of Cyclododecatriene from 1,3-Butadiene by Trimerization over Amine-Titanium Complex Catalyst (아민-티타늄착체 촉매상에서 1,3-부타디엔의 삼량화반응에 의한 싸이클로도데카트리엔의 합성)

  • Park, Da Min;Kim, Gye-Ryeong;Lee, Ju Hyun;Cho, Deuk Hee;Kim, Geon-Joong
    • Korean Chemical Engineering Research
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    • v.51 no.3
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    • pp.394-402
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    • 2013
  • The new complex catalysts were synthesized by the reaction of titanium compounds (titanium chloride or titanium butoxide) and diamines in this work, and they showed very high catalytic activities for the cyclododecatriene (CDT) synthesis from 1,3-butadiene through trimerization. CDT synthetic reaction was performed in an autoclave reactor, and the effects of reaction temperature, type of catalyst, catalyst amount added into the system, the mole ratio of Al/Ti and immobilization method were investigated on the yield of product CDT. The titanium complex catalyst combined to diamine with 1:1 ratio showed high selectivity to CDT more than 90%. The ratio of TTT-CDT/TTC-CDT isomers in the product revealed as different values, depending on the type of diamine combined to titanium and Ti/diamine ratios. Those homogeneous complexes could be used as a heterogenized catalyst after anchoring on the supports, and the immobilized titanium catalyst retained the catalytic activities for several times in the recycled reactions without leaching. The carbon support containing titanium has exhibited superior activity to the silica support. Especially, when the titanium complex was anchored on the support which was fabricated by the hydrolysis of tripropylaminosilane itself, the resulting titanium catalyst showed the highest BD conversion and CDT selectivity.

Development of a Simultaneous Analytical Method for Determination of Herbicide Fenquinotrione and KIH-3653-M-2 Residues in Agricultural Crops using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 제초제 fenquinotrione 및 대사산물 KIH-3653-M-2 동시시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.242-250
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    • 2019
  • An analytical method was developed for the determination of fenquinotrione, a triketone herbicide, in agricultural products. Fenquinotrione was metabolized to KIH-3653-M-2 in plants. Analyte extraction was conducted using 2% formic acid in acetonitrile and cleaned up using a hydrophillic-lipophillic balance (HLB) cartridge. The limits of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. Matrix-matched calibration curves were linear over the calibration ranges ($0.001{\sim}0.1{\mu}g/mL$) into a blank extract with $r^2>0.99$. The recovery results for fenquinotrione and KIH-3653-M-2 ranged between 81.1 to 116.2% and 78.0 to 110.0% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$) with relative standard deviation (RSD) less than 4.6%. All values were corresponded with the criteria ranges requested in both the Codex (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of fenquinotrione in the Republic of Korea.