• Title/Summary/Keyword: Sample matrix

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Research of Matrix Effect Reduction of $CsX^+$ SNMS ($CsX^+$ SNMS의 Matrix Effect 감소연구)

  • 문환구;김동원;한철현;김영남;심태언
    • Journal of the Korean Vacuum Society
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    • v.1 no.1
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    • pp.115-120
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    • 1992
  • SIMS is an indispensable surface analysis instrument in trace element depth profiling because of high detection sensitivity and excellent depth resolution, however, it requires a standard sample to do quantitative analysis due to matrix effect depending on the species of impurities and sample matricies and on the sputtering rates. Among the SNMS technology developed to supply the deficiency, we researched into CsX+ SNMS which improved the result quantitatively without any extra epuipments. So basic SNMS functions were confirmed through matrix element composition rate analysis using Siq layer etc., and adaptability to trace element concentration alaysis was tried. For that purpose we compared SIMS depth profile data for Boron which presented strong matrix effect on account of Fluorin existence after BF2 ion implantation on silicon substrate with SNMS data. Also detection limit and dynamic range were investigated. After these experements we concluded that CsX+ SNMS reduced matrix effect and we could apply it to profile impurity elements.

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Matrix solid phase dispersion(MSPD) extraction and HPLC determination of enrofloxacin and ciprofloxacin in pork muscle tissue (시료고체상분산(matrix solid phase dispersion)전처리법과 액체크로마토그라피를 이용한 돈육중 enrofloxacin 및 ciprofloxacin 분석)

  • Kang, Hwan-goo;Son, Seong-wan;Lee, Hye-sook;Kim, Jae-hak;Cho, Myung-haing
    • Korean Journal of Veterinary Research
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    • v.37 no.1
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    • pp.195-202
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    • 1997
  • A method for the isolation by matrix solid phase dispersion method and liquid chromatographic determination of enrofloxacin and ciprofloxacin in pork muscle tissue is presented. Blank or enrofloxacin and ciprofloxacin spiked samples(0.5g) containing 0.05g oxalic acid were blended with $C_{18}$(octadecylsilyl derivatized silica) packing material. After homogenization, $C_{18}$/muscle tissue matrix was transferred to glass column made from 10ml glass syringe and filter paper, and compressed to 4~4.5ml volume. A column was washed with 8ml of hexane and dried under vacuum. Interfering materials were removed by ethylacetate 8ml and dried, following which enrofloxacin and ciprofloxacin were eluted with 8ml of methanal under gravity. The eluate containing enrofloxacin and ciprofloxacin wase free from interfering compound when analysed by HPLC with UV detection at 278nm. Enrofloxacin and ciprofloxacin showed linear response with UV detector at the range of $0.05{\sim}1.0{\mu}g/ml$ and eluted within 5ml elution volume of methanol from the matrix. Fortified sample containing 0.05g oxalic acid represented more good recoveries than that of control sample. Average percentages of enrofloxacin and ciprofloxacin were $93.30{\pm}4.56%$ and $91.84{\pm}4.17%$, respectively, for the concentration range(0.05, 0.1, 0.25, 0.5 and $0.75{\mu}g/g$). The interassay variability of enrofloxacin was $6.02{\pm}5.33%$ with an intra-assay variability of 4.89% and $6.75{\pm}2.68%$ with 4.54% for ciprofloxacin. Detection limit of enrofloxacin and ciprofloxacin was $0.030{\mu}g/g$ in the spiked sample.

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Optimization of Solid Phase Extraction Method for Quantitative Analysis of Perfluorooctanoic Acid in Serum using Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Hyun-Seok;Yim, Yong-Hyeon
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.30-33
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    • 2014
  • A solid phase extraction (SPE) method was optimized for the quantitative analysis of perfluorooctanoic acid (PFOA) in serum using hydrophilic-lipophilic balance SPE and LC-MS/MS. Fetal bovine serums spiked with $^{13}C_8$-PFOA before or after SPE were used as test samples for evaluation of the SPE efficiency. Simultaneous evaluation of matrix effects and absolute SPE recovery for $^{13}C_8$-PFOA in serum using different sample pre-treatments and SPE conditions allowed optimization of SPE process efficiency with minimal matrix effect and decent SPE recovery. Introduction of protein precipitation as a sample pre-treatment procedure for serum samples before SPE generally decreased matrix effect in LC-MS/MS analysis and provided more stable recovery of PFOA.

Analysis of Perchlorate in Water Using Ion Chromatograph with Preconcentration (이온크로마토그래프를 이용한 수중의 퍼클로레이트 농축 및 분석)

  • Kim, Hak-Chul
    • Journal of environmental and Sanitary engineering
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    • v.21 no.4 s.62
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    • pp.29-38
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    • 2006
  • This study included the development of analytical method for determining perchlorate in water sample. The analytical condition was referred in EPA 314.0 method which use ion chromatography and the concentrator column was replaced by the guard column. Concentrating 10mL raw or treated water sample on to AGl6 guard column made it possible to get the LOD(Limit of Detection) of $0.73\;{\mu}g/L$. The total run time was 11 minutes and during run time next sample could be concentrated on AGl6 guard column. Compared to the Concentration method which needed manual operation, the Direct Injection method could screen the many water samples. The LOD of the Direct Injection method was higher and the sensitivity was lower than that of the Concentration method. The RSDs(Relative Standard Deviations) were lower than 2.5 % for peak height and 0.7 % for retention time in pre-concentration methods. This method Showed good reproducibility and reliability and it was thought the deviations of recovery value could be reduced by considering column capacity and making water sample homogeneous. Matrix Elimination could be done using the pre-concentration method if perchlorate were in complex matrix of sample.

Characterizations of Two-step Matrix Application Procedures for Imaging Mass Spectrometry

  • Shimma, Shuichi
    • Mass Spectrometry Letters
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    • v.6 no.1
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    • pp.21-25
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    • 2015
  • In this paper, I describe the importance of matrix spraying conditions in imaging mass spectrometry (IMS) to obtain successful imaging results. My developed matrix application methodology, which is a "two-step matrix application" sequentially combined with matrix sublimation and spraying matrix solution can provide high reproducibility and high ion yield compared with a conventional direct spraying method. However, insufficient IMS results were obtained occasionally despite the two-step method. Therefore, I wanted to characterize the methodology to continuously provide high quality data. According to my results, the sublimation time was not a strict parameter, and the most important step was the first spraying condition. This means that the extraction conditions from the tissue section and co-crystallization of the matrix were the most important factors.

CsX+ SNMS의 Matrix Effect 감소연구

  • 문환구;김동원;한철현;김영남;심태언
    • Proceedings of the Korean Vacuum Society Conference
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    • 1992.02a
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    • pp.17-18
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    • 1992
  • SIMS is an indispensable surface analysis instrument in trace element depth p profiling because of high detection sensitivity and excellent depth r resolution, however, it requires standard sample to do quantitative analysis d due to matrix effect depending on the species of impurities and sample m matricies and on the sputtering rates. A Among the SNMS technology developed to supply the deficiency, we researched i into CsX+ SNMS which improved the resul t quanti tati vely wi thout any extra epuipments. So basic SNMS functions were confirmed through matrix element composition rate a analysis using Si02 layer etc. and adaptability to trace element c concentration analysis was tried. For that purpose we compared SIMS depth profile data for Boron which presented s strong matrix effect on account of Fluorin existence after BF2 ion implantation on silicon substrate with SNMS data. d dynamic range were investigated. A After these experements we concluded that CsX+ SNMS reduced matrix effect and we could apply it to profile impurity elements.

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CUSUM Chart to Monitor Dispersion Matrix for Multivariate Normal Process

  • Chang, Duk-Joon;Kwon, Yong-Man;Hong, Yeon-Woong
    • 한국데이터정보과학회:학술대회논문집
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    • 2003.05a
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    • pp.89-95
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    • 2003
  • Cumulative sum(CUSUM) control charts for monitoring dispersion matrix under multivariate normal process are proposed. Performances of the proposed CUSUM charts are measured in terms of average run length(ARL) by simulation. Numerical results show that small reference values of the proposed CUSUM chart is more efficient for small shifts in the production process.

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Effects of Tungsten Addition on Tensile Properties of a Refractory Nb-l8Si-l0Ti-l0Mo-χW (χ=0, 5, 10 and 15 mot.%) In-situ Composites at 1670 K

  • 김진학;Tatsuo Tabaru;Hisatoshi Hirai
    • Transactions of Materials Processing
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    • v.8 no.3
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    • pp.233-233
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    • 1999
  • To investigate the effect of tungsten addition on mechanical properties, we prepared refractory (62χ)Nb-18Si-l00Mo-l0Ti-χW (χ=0, 5, 10 and 15 mol.%) in-situ composites by the conventional arc-casting technique, and then explored the microstructure, hardness and elastic modulus at ambient temperature and tensile properties at 1670 K. The microstructure consists of relatively fine (Nb, Mo, W, Ti)/sub 5/Si₃, silicide and a Nb solid solution matrix, and the fine eutectic microstructure becomes predominant at a Si content of around 18 mol.%. The hardness of (Nb, Mo, W, Ti(/sub 5/Si₃, silicide in a W-free sample is 1680 GPa, and goes up to 1980 GPa in a W 15 mol.% sample. The hardness, however, of Nb solid solution does not exhibit a remarkable difference when the nominal W content is increased. The elastic modulus shows a similar tendency to the hardness. The optimum tensile properties of the composites investigated are achieved at W 5 mol.% sample, which exhibits a relatively good ultimate strength of 230 MPa and an excellent balance of yield strength of 215 MPa, and an elongation of 3.7%. The SEM fractography generally indicates a ductile fracture in the W-free sample, and a cleavage rupture in W-impregnated ones.

Comparison between Head Space Gas Sampling and Purge & Trap Sampling in Water Analysis

  • Nagayanagi, Yutaka;Nakagawa, Katsuhiro;Saito, Yoshihiro;Kim, Poongzag
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.739-744
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    • 1995
  • The two main methods to prepare water samples for analyzing volatile organic compounds(VOC's) were investigated. One is the purge and trap(PT) method and another is the head space(HS) sampling method. Both methods were effective to transfer the low boiling point components from the water sample onto the capillary column. The cryo-focusing at the top of the main capillary column was an effective way to obtain the sharpness of the chromatographic peaks but could be avoided when a semi-wide bore column was used. The recovery from the same amount of the sample was better in PT than in HS but a larger sample volume in HS method could compensate the lower efficiency. Therefore PT is suitable to the analysis of drinking water where the very low concentration must be determined. HS is suitable to waste water analysis because of the easiness of the operation. The repeatability was good and similar in both methods. For the contamination of the former sample, both methods were tough and could be used without any problems. The matrix effect which could change the equilibrium parameters in HS method was find negligible in many components. The actual samples such as tap water and river water were analyzed with both methods concerning 16 components regulated in Korea.

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Isotachophoretically Assisted On-Line Complexation of Trace Metal Ions in a Highly Saline Matrix for Capillary Electrophoresis

  • Kim, Ji-Hye;Choi, Ki-Hwan;Cho, Sun-Young;Riaz, Asif;Chung, Doo-Soo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.3
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    • pp.790-794
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    • 2012
  • Trace metal ions such as $Cd^{2+}$, $Ni^{2+}$, and $Zn^{2+}$ in a highly saline sample were subjected to on-line complexation with 4-(2-thiazolylazo) resorcinol (TAR) dissolved in a background electrolyte (BGE) under transient isotachophoresis (TITP) conditions. A long plug of the saline sample, containing the trace metal ions but devoid of TAR, was injected into a coated capillary filled with a BGE composed of 150 mM 2-(cyclohexylamino) ethanesulfonic acid (CHES) and 110 mM triethylamine (TEA) at pH 9.7. Since the electrophoretic mobility of TAR fell between the mobilities of the anionic leading electrolyte ($Cl^-$ in the sample) and the anionic terminating background electrolyte ($CHES^-$), a highly concentrated zone of TAR from the BGE was formed at the rear of the sample matrix and then the metal cations toward the cathode were swept by isotachophoretically assisted on-line complexation (IAOC) between the metal ions and the isotachophoretically stacked TAR. As a result, anionic metal-TAR complexes were formed efficiently, which satisfy the TITP conditions between $Cl^-$ and $CHES^-$. The enrichment factors of metal ions including $Cd^{2+}$ were up to 780-fold compared to a conventional CZE mode using absorbance detection. The detection limits were 17 nM, 15 nM, and 27 nM for $Ni^{2+}$, $Zn^{2+}$, and $Cd^{2+}$ in a 250 mM NaCl matrix, respectively. Our method was successfully applied to the analysis of urine samples without desalting.