• Title/Summary/Keyword: Ion extraction

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High Speed Separation of PFCs in Human Serum by C18-Monolithic Column Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Won-Woong;Lee, Sun-Young;Yu, Se Mi;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • v.33 no.11
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    • pp.3727-3734
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    • 2012
  • An analytical method has been developed for the rapid determination of perfluorinated compounds (PFCs) in human serum samples. The extraction and purification of PFCs from human serum were performed by the modified method of previous report. Ten PFCs were rapidly separated within 3.3 min by C18-monolithic column liquid chromatography (LC) and detected by electrospray ionization (ESI) tandem mass spectrometry (MS/MS) in negative ion mode. The runtime of PFCs on monolithic column LC was up to 4-fold faster than that on conventional column LC. The effect of triethylamine (TEA) to the mobile phase has investigated on the overall MS detection sensitivity of PFCs in ESI ionization. Quantification was performed by LC-MS/MS in multiple-ion reaction monitoring (MRM) mode, using $^{13}C$-labeled internal standards. Method validation was performed to determine recovery, linearity, precision, and limits of quantification, followed by, the analysis of a standard reference material (SRM 1957 from NIST). The overall recoveries ranged between 81.5 and 106.3% with RSDs of 3.4 to 16.2% for the entire procedure. The calibration range extended from 0.33 to 50 $ng\;mL^{-1}$, with a correlation coefficient ($R^2$) greater than 0.995 and the limits of quantification with 0.08 to 0.46 $ng\;mL^{-1}$. This approach can be used for rapid and sensitive quantitative analysis of 10 PFCs in human serum with high performance and accuracy.

Electrochemical Behaviors and Analytical Application of Copper-1,5,9,13-Tetrathiacyclohexadecane Complex in Acetonitrile (아세토니트릴 용매 중에서 Copper-1,5,9,13-Tetrathiacyclohexadecane착물의 전기화학적 거동과 그 분석적 응용)

  • Moo-Lyong Seo;Bu-Yong Lee;Myung-Ja Choi;Bae Jun Ung;Park Tae Myeong
    • Journal of the Korean Chemical Society
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    • v.36 no.3
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    • pp.412-418
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    • 1992
  • The electrochemical behaviors and analytical application of copper-1,5,9,13-tetrathiacyclohexadecane[16-ane-$S_4$] complex in acetonitrile(AN) solution have been investigated by the use of DC polarography and differential pulse polarography. Thus the formation constant of copper complex was $10^{3.51}$. Copper (Ⅱ) ion was found to form complex of 1-to-1 composition with [16-ane-$S_4$]. In addition, reduction step was irreversible and the reduction current was diffusion controlled. And the effect of concentration of the salting-out reagent and chelating agent and pH of aqueous phase on the determination of copper (Ⅱ) was investigated and diverse ion effect was discussed. By salting-out extraction technique, we can be determined until the concentration of copper (Ⅱ) of 60 ppb.

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Urinary Profiling of Endogeneous Estrogens Using GC/MS (GC/MS에 의한 뇨 중 내인성 에스트로겐의 Profiling)

  • Lee, Seon Hwa;Yang, Yoon Jung;Kim, Tae Wook;Paeng, Ki Jung;Chung, Bong Chul
    • Journal of the Korean Chemical Society
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    • v.41 no.4
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    • pp.186-197
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    • 1997
  • Estrogens, which play an important role in sex hormone and potential inhibitor of cancer cell proliferation were profiled for normal female and male. The nineteen endogeneous estrogens were simultaneously analyzed by selected ion monitoring method of GC/MS. Urinary estrogens were extracted by using Serdolit AD-2 resin, hydrolyzed with $\beta-glucuronidase/arylsulfatase$ from Helix pomatia, liquid-liquid extraction and quantitatively derivatized by MSTFA/TMSCl mixture in order to be detected on the GC/MS. The good quality-control data were obtained through the precision and accuracy test and the recovery range of them was 80.97∼97.81%. The Korean reference values of urinary estrogens were established and differences were found in normal female compared with normal male.

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Enhanced Si based negative electrodes using RF/DC magnetron sputtering for bulk lithium ion batteries

  • Hwang, Chang-Muk;Park, Jong-Wan
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.277-277
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    • 2010
  • The capacity of the carbonaceous materials reached ca. $350\;mAhg^{-1}$ which is close to theorestical value of the carbon intercalation composition $LiC_6$, resulting in a relatively low volumetric Li capacity. Notwithstanding the capacities of carbon, it will not adjust well to the need so future devices. Silicon shows the highest gravimetric capacities (up to $4000\;mAhg^{-1}$ for $Li_{21}Si_5$). Although Si is the most promising of the next generation anodes, it undergoes a large volume change during lithium insertion and extraction. It results in pulverization of the Si and loss of electrical contact between the Si and the current collector during the lithiation and delithiation. Thus, its capacity fades rapidly during cycling. We focused on electrode materials in the multiphase form which were composed of two metal compounds to reduce the volume change in material design. A combination of electrochemically amorphous active material in an inert matrix (Si-M) has been investigated for use as negative electrode materials in lithium ion batteries. The matrix composited of Si-M alloys system that; active material (Si)-inactive material (M) with Li; M is a transition metal that does not alloy with Li with Li such as Ti, V or Mo. We fabricated and tested a broad range of Si-M compositions. The electrodes were sputter-deposited on rough Cu foil. Electrochemical, structural, and compositional characterization was performed using various techniques. The structure of Si-M alloys was investigated using X-ray Diffractometer (XRD) and transmission electron microscopy (TEM). Surface morphologies of the electrodes are observed using a field emission scanning electron microscopy (FESEM). The electrochemical properties of the electrodes are studied using the cycling test and electrochemical impedance spectroscopy (EIS). It is found that the capacity is strongly dependent on Si content and cycle retention is also changed according to M contents. It may be beneficial to find materials with high capacity, low irreversible capacity and that do not pulverize, and that combine Si-M to improve capacity retention.

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Recovery of Pure Ni(II) Compound by Precipitation from Hydrochloric Acid Solution Containing Si(IV) (규소(IV)가 함유된 염산용액으로부터 침전법에 의한 고순도 니켈(II)화합물의 회수)

  • Moon, Hyun Seung;Song, Si Jeong;Tran, Thanh Tuan;Lee, Man Seung
    • Resources Recycling
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    • v.30 no.6
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    • pp.36-42
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    • 2021
  • Spent lithium-ion batteries are treated by reduction-smelting at high temperatures to recover valuable metals. Solvent extraction and precipitation of the HCl leaching solution of reduction-smelted metallic alloys resulted in a filtrate containing Ni(II) and a small amount of Si(IV). Adsorption and precipitation experiments were conducted to recover pure Ni(II) compounds from the filtrate. Si(IV) was selectively loaded onto polyacrylamide, but this method did not efficiently filter the solution due to an increase in viscosity. The addition of Na2CO3 as a precipitant to the filtrate led to the simultaneous precipitation of Ni(II) and Si(IV). However, it was possible to recover nickel oxalate with a purity higher than 99.99% by selectively precipitating Ni(II) with the addition of Na2C2O4 as a precipitant.

A Review on Lithium Recovery by Membrane Process (멤브레인 공정에 의한 리튬 회수에 대한 총설)

  • Kim, Esther;Patel, Rajkumar
    • Membrane Journal
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    • v.31 no.5
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    • pp.315-326
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    • 2021
  • Lithium ion battery (LIB) demands increase every year globally to reduce the burden on fossil fuels. LIBs are used in electric vehicles, stationary storage systems and various other applications. Lithium is available in seawater, salt lakes, and brines and its extraction using environmentally friendly and inexpensive methods will greatly relieve the pressure in lithium mining. Membrane separation processes, mainly nanofiltration (NF), is an effective way for the separation of lithium metal from solutions. Electrodialysis and electrolysis are other separation processes used for lithium separation. The process of reverse osmosis (RO) is already a well-established method for the desalination of seawater; therefore, modifying RO membranes to target lithium metals is an excellent alternative method in which the only bottleneck is the interfering presence of other metal elements in the solution. Selectively removing lithium by finding or developing suitable NF membranes can be challenging, but it is nonetheless an exciting area of research. This review discusses in detail about lithium recovery via nanofiltration, electrodialysis, electrolysis and other processes.

Synthesis of DMDBTDMA and determination of radiolysis products by GC/MS (DMDBTDMA의 합성 및 방사선 분해산물의 GC/MS 분석)

  • Yang, Han-Beom;Lee, Eil-Hee;Park, Gyo-Beom
    • Analytical Science and Technology
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    • v.21 no.5
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    • pp.403-411
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    • 2008
  • Dimethyldibutyltetradecylmalonamide (DMDBTDMA) extractant was used in a solvent extraction process for a radioactive liquid waste treatment. For the study of radiolysis phenomena, DMDBTDMA was synthesized and the degradation compounds (n-methylbutylamine, tetradecane, 1-tetradecanol) in the DMDBTDMA extractant, irradiated with $^{60}Co$ gamma ray, were identified and determined as radiolysis products by a Fourier transform infrared (FT-IR), gas chromatograph/mass spectrometer (GC/MS) analysis and GC/MS with selected ion monitoring (SIM) mode. Retention behavior of n-methylbutylamine, n-dodecane, tetradecane and 1-tetradecanol in the total ion chromatogram with the standard materials and n-dodecane as the internal standard (ISTD) were 2.35 min., 8.83 min., 10.68 min. and 12.75 min., respectively. In the case of tetradecane, there was a linear relationship between the concentration of the tetradecane and the absorbed dose of the ${\gamma}$-ray irradiated DMDBTDMA.

Analysis of Matrine Alkaloids in Human Urine by Hollow Fiber Liquid-phase Microextraction with High-performance Liquid Chromatography (고성능 액체 크로마토그래피의 중공섬유 액상 미세추출에 의한 인간뇨의 Matrine Alkaloids의 분석)

  • Han, Dan-Dan;Row, Kyung-Ho
    • Journal of the Korean Chemical Society
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    • v.54 no.1
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    • pp.38-42
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    • 2010
  • A sensitive quantitative method for the determination of matrine alkaloids in human urine was developed based on hollow fiber liquid-phase microextraction (HF-LPME) combined with HPLC. The influence of the different factors on the HF-LPME efficiency including the pH and ion strength of the donar solution, the pH of the acceptor solution, stirring rate and extraction time were examined. The best HF-LPME conditions were as follows: 1-octanol impregnated in the pores of the hollow fiber, 100 mmol/L of $H_3PO_4$ at pH 1.50 as the acceptor solution injected into the lumen of the hollow fiber, 1 mol/L NaOH used to adjust the pH of the donor solution, stirring rate of 600 rpm and extraction time of 60 min. The LPME method was applied successfully to the analysis of matrine and sophocarpine in real urine samples.

Performance of carbon fiber added to anodes of conductive cement-graphite pastes used in electrochemical chloride extraction in concretes

  • Pellegrini-Cervantes, M.J.;Barrios-Durstewitz, C.P.;Nunez-Jaquez, R.E.;Baldenebro-Lopez, F.J.;Corral-Higuera, R.;Arredondo-Rea, S.P.;Rodriguez-Rodriguez, M.;Llanes-Cardenas, O.;Beltran-Chacon, R.
    • Carbon letters
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    • v.26
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    • pp.18-24
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    • 2018
  • Pollution of chloride ion-reinforced concrete can trigger active corrosion processes that reduce the useful life of structures. Multifunctional materials used as a counter-electrode by electrochemical techniques have been used to rehabilitate contaminated concrete. Cement-based pastes added to carbonaceous material, fibers or dust, have been used as an anode in the non-destructive Electrochemical Chloride Extraction (ECE) technique. We studied the performance of the addition of Carbon Fiber (CF) in a cement-graphite powder base paste used as an anode in ECE of concretes contaminated with chlorides from the preparation of the mixture. The experimental parameters were: 2.3% of free chlorides, 21 days of ECE application, a Carbon Fiber Volume Fraction (CFVF) of 0.1, 0.3, 0.6, 0.9%, a lithium borate alkaline electrolyte, a current density of $4.0A/m^2$ and a cement/graphite ratio of 1.0 for the paste. The efficiency of the ECE in the traditional technique using metal mesh as an anode was 77.6% and for CFVF of 0.9% it was 90.4%, with a tendency to increase to higher percentages of the CFVF in the conductive cement-graphite paste, keeping the pH stable and achieving a homogeneous ECE in the mass of the concrete contaminated with chlorides.

Acid Property and Catalytic Activity on Mordenites Treated by Hydrochloric Acid and Hydrofluoric Acid (염산 및 불산처리 모더나이트의 산특성과 촉매활성)

  • Han, Young-Taek;Ha, Baik-Hyon
    • Applied Chemistry for Engineering
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    • v.2 no.1
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    • pp.77-85
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    • 1991
  • A series of samples having different $SiO_2/Al_2O_3$ ratio were prepared by treating hydrogen mordenites with boiling hydrochloric acid and with hydrofluoric acid. The acidities of these samples were measured by TPD of $NH_3$ and by pyridine adsorption using IR, and the catalytic activities and selectivities of isomerization were measured for the reaction of ortho-xylene. For the samples treated by boiling hydrochloric acid, the acidities decreased with the increasing $SiO_2/Al_2O_3$ ratio caused by the extraction of framework aluminum. The sample having the $SiO_2/Al_2O_3$ ratio or 22 showed better activity than the others. For the samples treated by hydrofluoric acid, the content of chemically binding fluorine increased with the increasing contact time of hydrofluoric acid solution. The catalytic activities decreased with the hydrofluoric acid treatment due to the decreased acid sites resulted from the extraction of aluminum and silicon as well as the hydroxyl group replacement by the fluoride ion. The slightly increasing catalytic activities, however, came from the newly created acid sites, due to the removal of surface silicon, having enhanced by the inductive effect of binding fluorin with further acid treatment.

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