• Title/Summary/Keyword: lM HCl extraction

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Some heavy metal concentration of surface sediments from the southwestern coast of Korea (서남해안 연근해저 퇴적물의 중금속 함량 및 분포)

  • 전수경;조영길
    • Journal of Environmental Science International
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    • v.11 no.12
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    • pp.1299-1305
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    • 2002
  • Thirty sediment samples of the <63${\mu}{\textrm}{m}$ fraction collected from the southwestern coast of Korea were analysed for their heavy metal (Fe, Mn, Cr, Co, Cu, Ni, Zn and Pb) concentration. The results show that sediment texture plays a controlling role on the total metal concentrations and their spatial distribution. A single lM HCl extraction procedure was used in order to assess the environmental risk of heavy metals in bottom sediments. The non-residual fraction was the most abundant pool for Mn and Pb in most samples, which means that this metals are highly avaliable in these sediments. Cr, Ni, Fe, Co, Zn and Cu were mainly associated with the residual fraction, suggesting that their concentrations are controlled significantly by transport processes with the fine particles as carriers from diffuse pollution source. Concentration enrichment ratios(CER) were calculated from the non-residual contents and their values allowed us to classify the sediments according to their environmental risk.

Regeneration of $FeCl_3$ from a Spent Etching Solution Containing Nickel by Solvent Extraction (니켈 함유 에칭폐액으로부터 용매추출에 의한 $FeCl_3$의 재생)

  • Lee, Kyoung-Joo;Lee, man-Seung;Oh, Young-Joo
    • Proceedings of the Korean Institute of Resources Recycling Conference
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    • 2004.05a
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    • pp.218-226
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    • 2004
  • Solvent extraction and stripping experiments were conducted to separate iron from a spent $FeCl_3$ etching solution containing nickel. In the extraction, PC88A, MIBK and Alamine336 were tested as an extractant in various diluents. Alamine336 salt in toluene led to the highest extraction percentage of iron. Stripping percentage of iron from the loaded organic by Alamine336 increased with decreasing HCl conentration of stripping solution and with increasing volume ratio of aqueous to organic. In the operation of bench scale mixer-settler, 7 extraction stage with 1.0M Alamine336 salt in toluene and 10 stripping stage with 0.01M HCl solution resulted in a stripped solution with 133g/L of iron and in a raffinate with most of nickel together with a small amount of iron when the flow rate ratio of organic to aqueous was 7.

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Determination of Corticosteroids in Moisturizers by LC-MS/MS

  • Park, Sumin;Choi, Gye Young;Lee, Seon-Ah;Kim, Hyun Jeong;Yum, Hye Yung;Paeng, Ki-Jung
    • Mass Spectrometry Letters
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    • v.7 no.1
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    • pp.26-29
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    • 2016
  • Simultaneous determination of three corticosteroids (clobetasol propionate, betamethasone dipropionate, fluticasone propionate) in moisturizers was performed by using liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS). Sample preparation was conducted by the liquid-liquid extraction (LLE). Moisturizers include emulsifying agent and it forms micelles. In order to improve the extraction efficiency of corticosteroids trapped in micelle, newly developed-optimized extraction conditions which can remove the matrix effect from moisturizers was applied with various pH conditions in LLE extraction stage of sample preparation. Thus, the addition of 10 μL of 1 M HCl into moisturizers sample before extraction could improve the extraction efficiency. For the quantitative analysis, SRM table that contained specific transition of all of target corticosteroids was created. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), limit of quantization (LOQ) and recovery. Over the 0.99 r2 value was obtained in calibration standard range. Effective accuracy and precision were also obtained. LODs were below 31 ng/mL and LOQs were estimated below 94 ng/mL for all corticosteroids tested.

The Optimization of Solvent Extraction Process of Iron Chloride Etching Waste Solution (염화철 에칭폐액의 용매추출공정 최적화에 관한 연구)

  • Park, Il-Jeong;Kim, Dae-Weon;Kim, Geon-Hong;Chae, Hong-jun;Lee, Sang-Woo;Jung, Hang-Chul
    • Clean Technology
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    • v.23 no.3
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    • pp.279-285
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    • 2017
  • In this study, a new organophosphorus acid-based solvent (KMC-P) from KMC Co., Ltd. was used for the recovery of the iron chloride etching waste solution. In order to increase the extraction efficiency for the new solvent in the solvent extraction process, we selected the process variables and conducted the optimization experiment according to the DOE to investigate the correlation between the variables. Solvent concentration, pH, and O/A ratio were found to be factors affecting extraction and stripping efficiency. The optimum stripping efficiency was 69.7% when the solvent concentration was 29.4 wt%, the HCl addition amount was 0 mL, and the O/A ratio was 7, and the reliability was more than 86%.

Determination of Mefenamic Acid in Human Urine by Means of Two Spectroscopic Methods by Using Cloud Point Extraction Methodology as a Tool for Treatment of Samples

  • Tabrizi, Ahad Bavili
    • Bulletin of the Korean Chemical Society
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    • v.27 no.11
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    • pp.1780-1784
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    • 2006
  • Cloud point extraction was used to extract mefenamic acid (MF) from human urine, and spectrofluorimetry and spectrophotometry were used to analyze extracted MF. The variables affecting extraction and phase separation, i.e. HCl and Triton X-114 concentration, temperature and time of equilibration, were optimized. Under the experimental conditions used the limit of detection for extraction of 25 mL of sample was 0.006 and 0.045 mg $L^{-1}$, with relative standard deviations of 2.52 and 1.45% (n = 5) for spectrofluorimetric or spectrophotometric methods, respectively. Good recoveries in the range of 95-107% were obtained for spiked samples. The proposed methods were applied to the determination of MF in human urine.

Separation of High Purity Terbium Using Extraction Chromatography (추출 크로마토그래피를 이용한 고순도 테르븀의 분리)

  • Lee, Kwang-Pill;Park, Myoung-Jin;Park, Keung-Shik;Lee, Hueng-Lark;Piao, Zhexiu
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.370-374
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    • 1999
  • Extraction chromatography was used to scarch optimum separation conditions of terbium. Stationary phase was 2-ethylhexyl-2-ethylhexyl phosphonic acid(HEH[EHP])levextrel (-100~+150 mesh), column size was ${\Phi}20{\times}530mm$ and kept constantly temperature at $50^{\circ}C$, adsorption flow rate of $0.2mL/cm^2{\cdot}min$, elution flow rate of $1.0mL/cm^2{\cdot}min$, column diameter to packing height of 1:15. But to search optimum separation conditions of terbium, it changed the eluent acidity, the loading weight of sample. the composition of sample. In conclusion, acidity was 0.6 N HCl, loading weight of sample was about 5% and composition of sample was $Gd_2O_3(20%)+Tb_4O_7(60%)+Dy_2O_3(20%)$. Moreover purity of separated terbium by ICP-AES analysis was 99.98% in yield of 99.99%.

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Colorimetric Determination of Trace Mercury(II) in Water by Back Extraction and PAR (역추출과 PAR법에 의한 수질중 미량 수은의 비색정량에 관한 연구)

  • 정창웅
    • Journal of Environmental Health Sciences
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    • v.21 no.3
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    • pp.96-101
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    • 1995
  • A selective and highly sensitive spectrophotometric measurements have been developed for the determination of trace mercury(II) with thiosulfate and PAR. Hg(II)-thiosulfate complex was extracted into high molecular alkylamine such as quaternary ammonium salt and back extracted into 1 M-HCl solution. The Hg(II)-PAR complex has maximum absorbance at 499 nm and obeys Beer's law in the range of 0.04~1.0 $\mu g/mL$ of mercury(II). The molar absorptivity and Sandell's sensitivity are $6.27\times 10^4 L.mole^{-1} cm^{-1}$ and $3.2\times 10^{-3}g/cm^2$ respectively.

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Determination of Persistent Organochlorine Pollutants in Rat Hair by Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang;Pyo, Hee-Soo;Park, Song-Ja
    • Bulletin of the Korean Chemical Society
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    • v.25 no.10
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    • pp.1489-1494
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    • 2004
  • A gas chromatography/mass spectrometric assay method was developed for the determination of persistent organochlorine pollutants (POPs) in hair. For the exact extraction study was used hair of rat exposed with POPs. Sonication of the hair matrix with 3 M HCl solution in methylene chloride of the extraction methods studied was the most efficient and rapid sample preparation method. After sonication of rat hair was achieved clean up with a solid phase extraction procedure using silica gel-florisil. Elution was performed with 8 mL of methylene chloride. The eluate was concentrated to approximately 100 ${\mu}L$ and analyzed by gas chromatography-mass spectrometry (GC-MS). Detection limits of POPs were in the concentration range of 0.6-1.2 ng/g in rat hair. Aldrin, dieldrin, p,p-DDT and mirex were dosed rat for 4 weeks at concentration of 0.01 mg/L in drinking water and detected in rat hair at concentration of 2.8, 11.3, 7.9 and 15.6 ng/g, respectively. Aldrin and p,p-DDT were metabolized to dieldrin and p,p-DDE, which were detected in concentration of 9.7 and 2.9 ng/g in rat hair, respectively. The developed method may be valuable to be used to analyze POPs in human hair.

Rapid Determination of L-carnitine in Infant and Toddler Formulas by Liquid Chromatography Tandem Mass Spectrometry

  • Ahn, Jang-Hyuk;Kwak, Byung-Man;Park, Jung-Min;Kim, Na-Kyeoung;Kim, Jin-Man
    • Food Science of Animal Resources
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    • v.34 no.6
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    • pp.749-756
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    • 2014
  • A rapid and simple analytical method for L-carnitine was developed for infant and toddler formulas by liquid chromatography tandem mass spectrometry (LC-MS/MS). A 0.3 g of infant formula and toddler formula sample was mixed in a 50 mL conical tube with 9 mL water and 1 mL 0.1 M hydrochloric acid (HCl) to chemical extraction. Then, chloroform was used for removing a lipid fraction. After centrifuged, L-carnitine was separated and quantified using LC-MS/MS with electrospray ionization (ESI) mode. The precursor ion for L-carnitine was m/z 162, and product ions were m/z 103 (quantitative) and m/z 85 (qualitative), respectively. The results for spiked recovery test were in the range of 93.18-95.64% and the result for certified reference material (SRM 1849a) was within the range of the certificated values. This method could be implemented in many laboratories that require time and labor saving.

A Selective Determination Method of Inorganic and Organic Mercury (무기수은과 유기수은의 선택정량)

  • Kim, Chon Han
    • Journal of the Korean Chemical Society
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    • v.41 no.8
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    • pp.392-398
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    • 1997
  • A method of selective determination of inorganic and organic mercury compounds has been described. The $CHCl_3$ solution of a high molecular quaternary alkylammonium salt, Aliquat 336 was used for the simultaneous preconcentration of both inorganic, $Hg^{2+}$ as its thiocyanate complex, and organic mercury compounds, $CH_3HgCl$ and $C_2H_3O_2$ $HgC_6H_5$ by extraction from their aqueous solution. Selective separation of the inorganic mercury from the extract was followed by stripping with 3 M $HClO_4 $ solution for the subsequent determination by CVAAS. Organic mercury was also determined by CVAAS after removal of $CHCl_3solvent$ from the extract and decomposition of the residue with 4% $KMnO_4 $-1 MH_2$S0_4$. The mixtures of inorganic and organic mercury compounds contained 1.0 $\mug$ as Hg in 50 mL of sample solution(0.02 ${\mu}gHg/mL$) were analysed within ${\pm}6%$ by absolute errors.

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