• Title/Summary/Keyword: Solid-phase reagent

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Application of Polyurethane Foam Loaded with a Schiff Base Ligand for Determination of Trace Amounts of Copper in Water Samples by Flame Atomic Absorption Spectroscopy

  • Moftakhar, Mahdieh Koorehpazan;Yaftian, Mohammad Reza;Nahaei, Samaneh;Zamani, Abbas Ali
    • Journal of the Korean Chemical Society
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    • v.58 no.3
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    • pp.283-288
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    • 2014
  • A column solid phase extraction procedure based on modified polyurethane foam (PUF) by a newly synthesized Schiff base ionophore, named 2,2'-{iminobis[propane-3,1-diylnitrilo(1E)prop-1-yl-1-ylidene]}diphenol, was developed for preconcentration step of trace amounts determination of copper ions in water samples by atomic absorption flame spectroscopy. The influence of parameters on the adsorption process such as sample pH, amount of modified PUF packed in the column, type and volume of stripping reagent and its flow rate were investigated and optimized. Under optimum experimental conditions, the calibration graph was linear in a relatively wide range ($0.005-210{\mu}g/ml$) with a limit of detection $0.002{\mu}g/ml$ of copper. The proposed method allows achieving to a concentration factor of >133. The capacity of a column (1.6 cm i.d.) packed by 6 g of PUF modified by 12 mg of the Schiff base was found to be $247.7({\pm}2.1){\mu}g$ of copper. It was found that the adsorption process was highly selective towards copper ions with respect to some associated metal ions. The presented procedure was successfully applied for determination of copper in some water samples.

The Analysis of Airborne Trimethylamine Using a Headspace (HS)-SPME Method (헤드스페이스-SPME 방법을 이용한 트리메틸아민의 분석방법 연구)

  • Ahn, Ji-Won;Kim, Ki-Hyun
    • Journal of Korean Society for Atmospheric Environment
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    • v.24 no.3
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    • pp.357-366
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    • 2008
  • In this study, the analytical performance of trimethylamine (TMA) were investigated with respect to headspace-solid phase microextraction (HS-SPME) method. In order to induce the elution of aqueous TMA to headspace, NaOH was added as a decomposition reagent to aqueous TMA standard. By controlling the combination of three major variables for TMA extraction, the extent of extraction was compared between the two contrasting conditions for each variable (i.e., reaction time (long (L) vs short (S)), exposure temperature (30 vs $50^{\circ}C$), and exposure time (10 vs 30 min)). The results of this comparative analysis showed that the extraction efficiency for all eight types of HS-SPME combinations decreased on the order: L-30-30>L-50-10>L-30-10>L-50-30>S-30-30>S-50-30>S-50-10>S-30-10. The effect of reaction time appeared to exert significant influences on the relative recovery rate of HS-SPME at 90% confidence level. However, the effects of exposure temperature or exposure time were not so significant as reaction time. When the recovery rate of HS-SPME is compared against the direct injection of liquid standard into GC injector, it recorded as 2%. According to this comparative study, the reaction conditions for HS-SPME application can exert significant influences on the analysis of TMA.

Preconcentration, Separation and Determination of lead(II) with Methyl Thymol Blue Adsorbed on Activated Carbon Using Flame Atomic Absorption Spectrometry (불꽃원자 흡수 분광법으로 활성탄소에 흡착된 메틸티몰 블루로 납(II)의 예비농축, 분리 및 측정)

  • Ensafi, Ali A.;Ghaderi , Ali R.
    • Journal of the Korean Chemical Society
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    • v.52 no.1
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    • pp.16-22
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    • 2008
  • on-line system for preconcentration and separation of lead(II) is presented. The method is based on the complex formation of Pb(II) with adsorbed Methyl thymol blue on activated carbon. The conditions of preparing the solid phase reagent and of quantitative recovery of Pb(II) from diluted solutions, such as acidity of aqueous phase, solid phase capacity, and flow variables were studied as well as effect of potential interfering ions. After preconcentration step, the metal ions are eluted automatically by 5 ml of 0.5 M HNO3 solution and the lead ions content was determined by flame atomic absorption spectrometry. Under the optimum conditions, the lead ions in aqueous samples were separated and preconcentrated about 1000-fold by the column. The detection limit was 0.001 g mL-1. Lead has been determined in river and tap water samples, with recovery of 98 to 102%.

Alternative Immunossays

  • Barnard, G.J.R.;Kim, J.B.;Collins, W.P.
    • Korean Journal of Animal Reproduction
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    • v.9 no.2
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    • pp.133-139
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    • 1985
  • An immunoassay may be defined as an analytical procedure involving the competitive reaction between a limiting concentration of specific antibody and two populations of antigen, one of which is labelled or immobillized. The advent of immunoassay has revolutionised our knowledge of reproductive physiology and the practice of veterinary and clinical medicine. Radioimmunoassay (RIA) was the first of these methods to be developed, which meausred the analyte with good sensitivity, accuracy and precision (1,2). The essential components of RIA are:-(i) a limited concentration of antibodies, (ii) a reference preparation, and (iii) an antigen labelled with a radioisotope (usually tritium or iodine-125). Most procedures invelove isolating the antibody-bound fraction and measuring the amount of labelled antigen. Good facilities are available for scintilltion counting, data reduction nd statistical analysis. RIA is undergoing refinement through:-(i) the introduction of new techniques to separate the antibody-bound and free fractions which minimize the misclassification of labelled antigen into these compartments, and the amount of non-specfic binding. (3), (ii) the development of non-extration for the measurement of haptens (4), (iii) the determination of a, pp.rent free (i.e. non-protein bound) analytes (5), and (iv) the use of monoclonal antibodies(6). In 1968, Miles and Hales introduced in important new type of immunoassay which they termed immunora-diometric assay (IRMA) based on t도 use of isotopically labelled specific antibodies(7) in a move from limited to excess reagent systems. The concept of two-site IRMAs (with a capture antibody on a solid-phase, and a second labelled antibody to a different antigenic determinant of the analyte) has enabled the development of more sensitive and less-time consuming methods for the measurement of protein hormones ovar wide concentration of analyte (8). The increasing use of isotopic methos for diverse a, pp.ications has exposed several problems. For example, the radioactive half-life and radiolysis of the labelled reagent limits assay sensitivity and imposes a time limit on the usefulness of a kit. In addition, the potential health hazards associated with the use and disposal of radioactive cmpounds and the solvents and photofluors necessary for liquid scientillation counting are incompatable with the development of extra-laboratory tests. To date, the most practical alternative labels to radioisotopes, for the measurement of analytes in a concentration > 1 ng/ml, are erythrocytes, polystyrene particiles, gold sols, dyes and enzymes or cofactors with a visual or colorimetric end-point(9). Increased sensitivity to<1 pg/ml may be obtained with fluorescent and chemiluminescent labels, or enzymes with a fluorometric, chemiluminometric or bioluminometric end-point. The sensitivity of any immunoassay or immunometric assay depends on the affinity of the antibody-antigen reaction, the specific activity of the label, the precision with which the reagents are manipulated and the nonspecific background signal (10). The sensitivity of a limited reagent system for the measurement of haptens or proteins is mainly dependent upon the affinity of the antibodies and the smalleest amount of reagent that may be manipulated. Consequently, it is difficult in practice to improve on the sensitivity obtained with iodine-125 as the label. Conversely, with excess reagent systems for the measurement of proteins it is theoretically possible to increase assay sensitivity at least 1000 fold with alternative luminescent labels. To date, a 10-fold improvement has been achieved, and attempts are being made to reduce the influence of other variables on the specific signal from the immunoreaction.

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Preconcentration of Iron(III), Lead(II), Cobalt(II) and Chromium(III) on Amberlite XAD-1180 Resin Loaded with 4-(2-Pyridylazo)-resorcinol (PAR) and Their Determination by FAAS

  • Tokalloglu, Serife;Kartal, Senol
    • Bulletin of the Korean Chemical Society
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    • v.27 no.9
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    • pp.1293-1296
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    • 2006
  • In this study, a solid phase extraction method has been developed for the preconcentration and separation of the elements Cr(III), Fe(III), Co(II) and Pb(II) at trace levels by using a column packed with Amberlite XAD-1180 resin loaded with 4-(2-pyridylazo)-resorcinol (PAR) reagent. After preconcentrating, the metals retained on the column were eluted with 20 mL of 3 mol/L $HNO_3$ and then determined by flame atomic absorption spectrometry (FAAS). The factors affecting the recovery of the elements, such as pH, type and concentration of eluent, volume of sample and elution solution, and matrix components, were also ascertained. The recoveries of Cr(III), Fe(III), Co(II) and Pb(II) were found to be $99\;{\pm}\;4,\;97\;{\pm}\;3,\;95\;{\pm}\;3$ and $98\;{\pm}\;4$%, respectively, under the optimum conditions at 95% confidence level and the relative standard deviations found by analyzing of nine replicates were $\leq4.4$%. The preconcentration factors for Cr(III), Fe(III), Co(II) and Pb(II) were found as 75, 125, 50 and 75 respectively. The detection limits (DL, 3s/b) were 3.0 $\mu g/L$ for Cr(III), 1.25 $\mu g/L$ for Fe(III), 3.3 $\mu g/L$ for Co(II), and 7.2 $\mu g/L$ for Pb(II). The recoveries achieved by adding of metals at known concentrations to samples and the analysis results of Buffalo river sediment (RM 8704) show that the described method has a good accuracy. The proposed method was applied to tap water, stream water, salt and street dust samples.

Effect of Additives on Densification and Grain Growth of Magnesia (마그네시아의 치밀화 및 입자성장에 미치는 첨가물의 영향)

  • Lee, Hae-Weon;Kim, Whan
    • Journal of the Korean Ceramic Society
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    • v.19 no.2
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    • pp.127-132
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    • 1982
  • This experiment has been carried out for the purpose of investigating the effect of additives on densification and grain growth in magnesium oxide by a two-step process; hot pressing and heat treating. MgO powder has been obtained by calcining extra reagent grade MgCO3 at 90$0^{\circ}C$ for 30 minutes, and additives have been added to $MgCO_3$ in the form of soluble salts-Al$(NO_3)_3$$. $9H_2O$ and $Cr(NO_3)_3$.9H_2O$. The hot pressing has been carried out with changes of soaking time at 125$0^{\circ}C$ under the pressure of 250kg/$\textrm{cm}^2$, and the heat treating also at same temperature. The initial particle size of MgO measured by particle size analyzer was 0.86 microns. Densification rate obeyed the equation D=K lnt + C, and grain growth rate obeyed the equation G-G0=kt1/2. It was vaporization of some $Cr_2O_3$ and formation of solid solution that had an influence on desification of MgO containing $Cr_2O_3$. Activation energy for grain growth of pure MgO was 62.4 kcal/mole, therefore grain growth was supposed to be diffusioncontrolled process. But after heat treatmeat, excess additives were expected to slow down the grain growth by the formation of second phase or the solute atoms at grainboundary.

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Synthesis and Characterization of a Receptor-Targeting Contrast Agent

  • Yang, Taegyun;Park, Ji-Hyung;Lee, Seung-Cheol;Kim, Cheol-Su;Cho, Jee-Hyun;Lee, Chul-Hyun;Cheong, Chae-Joon
    • Journal of the Korean Magnetic Resonance Society
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    • v.7 no.1
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    • pp.46-54
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    • 2003
  • We synthesized a contrast agent for MRI that is capable of binding to the ABP-1 receptor and enhancing the contrast of the targeted cells. We used a lysine dendrimer (G=3)DTPA[Gd] as the contrast agent and synthesized a biotinylated polyclonal antibody for ABP-1 as the first antibody. Lysine dendrimers were prepared using the solid phase peptide synthesis method.$^3$ Amino-terminated lysine dendrimers were then coupled to DTPA using the anhydride method. Gd was complexed with the DTPA-lysine dendrimer in an acidic solution of 3 eq GdCl$_3$ to one of DTPA. The lysine dendrimer-DTPA[Gd] and avidin were conjugated in MES solution, pH 6.0, using EDC as the coupling reagent. The biotin-avidin system was used to link the polyclonal antibody and contrast agent. K562 cells were used for imaging.

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Quantitative Immunoassay for Polychlorinated Biphenyl Compounds in Electrical Insulating Oils

  • Kim In Soo
    • Proceedings of the Microbiological Society of Korea Conference
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    • 2000.10a
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    • pp.119-127
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    • 2000
  • The development and performance of a competitive indirect immunoassay for the quantitative measurement of polychlorinated biphenyl compounds in insulating oils is presented. Reagent preparation and the assay characterisation, optimisation and validation steps are described. The dynamic range of the assay for Aroclors 1254 and 1260 in methanol was $50-800 {\mu}g\;ml^{-1}$ with $50\%$ signal inhibition values of 217 and $ 212 {\mu}g\;ml^{-1}$ respectively. Impending legislation in the UK is likely to decree that oils containing $ >50 {\mu}g\;ml^{-1}$ PCB be considered contaminated. Assay sensitivity increased with the degree of PCB chlorination. The assay of structurally related compounds of environmental concern yielded cross-reactivity values of under $0.6\%$. The immunoassay proved reliable for the analysis of transformer oils containing $>70{\mu}g\;ml^{-1}$ PCB, but over-estimated PCB levels in oils containing $<20{\mu}g\;ml^{-1}$ of the analyte with the oils requiring pre-treatment using either solid-phase extraction techniques or washing with KOH-ethanol/sulphuric acid to remove matrix interferents. The analytical performance of the assay was compared against a commercially available semi-quantitative immunoassay kit for PCBs in soil and water.

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An Integrated Air Monitoring Approach for Assessment of Formaldehyde in the Workplace

  • Dugheri, Stefano;Bonari, Alessandro;Pompilio, Ilenia;Colpo, Marco;Mucci, Nicola;Arcangeli, Giulio
    • Safety and Health at Work
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    • v.9 no.4
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    • pp.479-485
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    • 2018
  • The aim of this study is to validate an integrated air monitoring approach for assessing airborne formaldehyde (FA) in the workplace. An active sampling by silica gel impregnated with 2,4-dinitrophenylhydrazine, a passive solid phase microextraction technique using O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine as on-fiber derivatization reagent, an electrochemical direct-reading monitor, and an enzyme-based badge were evaluated and tested over a range of 0.020-5.12 ppm, using dynamically generated FA air concentrations. Simple linear regression analysis showed the four methods were suitable for evaluating airborne FA. Personal and area samplings in 12 anatomy pathology departments showed that the international occupational exposure limits in the GESTIS database were frequently exceeded. This monitoring approach would allow a fast, easy-to-use, and economical evaluation of both current work practices and eventual changes made to reduce FA vapor concentrations.

Properties of the Ceramic Composites and Glass-Ceramics Prepared by Using the Natural Hydroxyapatite Derived from Tuna bone (참치 뼈에서 추출한 천연 Hydroxyapatite를 이용한 세라믹 복합체 및 Glass-Ceramics의 특성)

  • Choi, Jin-Sam;Lee, Chang-Kook;Jeon, You-Jin;Byun, Hee-Guk;Kim, Se-Kwon
    • Applied Chemistry for Engineering
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    • v.10 no.3
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    • pp.394-399
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    • 1999
  • As the prosthetic application of natural mineral substituted for chemical reagent, composites and a glass-ceramics containing hydro-xyapatite isolated from tuna bone were prepared by solid state reaction. On x-ray examinations, the major phases of composites were identified as pseudowollastonite(${\alpha}-CaSiO_3$) and ${\beta}$-tricalcium phosphate($\beta$-TCP) and the phase of a glass-ceramics was observed as $\beta$-TCP and fluoroapatite caused by $CaF_2$ respectively. SEM images depict that the microstructures of grain at the composites were a function of temperature. The measured strength of a glass-ceramics prepared at $900^{\circ}C$ for 4 hr in air was 90 MPa as a 4-point bending method and this value was similar to the cortical bone, as 50~150 MPa but it was lower than its maximum strength.

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