• Title/Summary/Keyword: laser ablation. ICP-MS

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Tandem laser-induced breakdown spectroscopy laser-ablation inductively-coupled plasma mass spectrometry analysis of high-purity alumina powder

  • Lee, Yonghoon;Kim, Hyang
    • Analytical Science and Technology
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    • v.32 no.4
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    • pp.121-130
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    • 2019
  • Alumina is one of the most important ceramic materials because of its useful physical and chemical properties. Recently, high-purity alumina has been used in various industrial fields. This leads to increasing demand for reliable elemental analysis of impurities in alumina samples. However, the chemical inertness of alumina makes the sample preparation for conventional elemental analysis a tremendously difficult task. Herein, we demonstrated the feasibility of laser ablation for effective sampling of alumina powder. Laser ablation performs sampling rapidly without any chemical reagents and also allows simultaneous optical emission spectroscopy and mass spectrometry analyses. For six alumina samples including certified reference materials and commercial products, laser-induced breakdown spectroscopy (LIBS) and laser-ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) analyses were performed simultaneously based on a common laser ablation sampling. LIBS was found to be useful to quantify alkali and alkaline earth metals with limits-of-detection (LODs) around 1 ppm. LA-ICP-MS could quantify transition metals such as Ti, Cu, Zn, and Zr with LODs in the range from a few tens to hundreds ppb.

SHIELDED LASER ABLATION ICP-MS SYSTEM FOR THE CHARACTERIZATION OF HIGH BURNUP FUEL

  • Ha, Yeong-Keong;Han, Sun-Ho;Kim, Hyun-Gyum;Kim, Won-Ho;Jee, Kwang-Yong
    • Nuclear Engineering and Technology
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    • v.40 no.4
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    • pp.311-318
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    • 2008
  • In modem power reactors, nuclear fuels have recently reached 55,000 MWd/MtU from the initial average burnup of 35,000 MWd/MtU to reduce the fuel cycle cost and waste volume. At such high burnups, a fuel pellet produces fission products proportional to the burnup and creates a typical high burnup structure around the periphery region of the pellet, producing the so called 'rim effect'. This rim region of a highly burnt fuel is known to be ca. $200\;{\mu}m$ in width and is known to affect the fuel integrity. To characterize the local burnup in the rim region, solid sampling in the micro meter region by laser ablation is needed so that the distribution of isotopes can be determined by ICP-MS. For this procedure, special radiation shielding is required for personnel safety. In this study, we installed a radiation shielded laser ablation ICP-MS system, and a performance test of the developed system was conducted to evaluate the safe operation of instruments.

Comparison Study of Sensitivity Factors of Elements in Glow Discharge- & Inductively Coupled Plasma- Mass Spectrometry

  • Kim, Young-Sang;Plotnikov, M.;Hoffmann, Volker
    • Bulletin of the Korean Chemical Society
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    • v.26 no.12
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    • pp.1991-1995
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    • 2005
  • Sensitivity factors of elements by a glow discharge mass spectrometry (GD-MS) were intensively investigated and compared with a laser ablation inductively coupled plasma-mass spectrometry (ICP-MS). In case of copper matrix, the sensitivity factor by GD-MS generally decreases with the increase of the mass number of element. The details are a little different between each data measured by Faraday and multiplier detectors. The factor by a multiplier detector drastically decreases with the mass increase in the region of low mass as in Faraday detector’s case, but slowly in the high mass region. On the contrast, the sensitivity factor of solution standard by a conventional ICP-MS slowly increases with the increase of elemental mass number even though there are some exceptions such as gold and also the sensitivity factor by a laser ablation ICP MS generally increases with mass number of element in the specimen of glass type. In case of steel matrix, any definite trends could not be shown in the relationship between the GD-MS’s sensitivity factor and elemental mass.

Preparation of Metal-p-aminobenzyl-DOTA Complex Using Magnetic Particles for Bio-tagging in Laser Ablation ICP-MS

  • Yoon, S.Y.;Lim, H.B.
    • Bulletin of the Korean Chemical Society
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    • v.33 no.11
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    • pp.3665-3670
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    • 2012
  • Metal-p-$NH_2$-Bn-DOTA (paraammionobenzyl-1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid: ABDOTA) complex was synthesized and purified for bio-tagging to quantify biological target materials using laser ablation (LA)-ICP-MS. Since the preparation of a pure and stable tagging complex is the key procedure for quantification, magnetic particles were used to purify the synthesized metal-ABDOTA complex. The magnetic particles immobilized with the complex attracted to a permanent magnet, resulting in fast separation from free un-reacted metal ions in solution. Gd ions formed the metal-complex with a higher yield of 64.3% (${\pm}3.9%$ relative standard deviation (RSD)) than Y ions, 52.3% (${\pm}2.5%$ RSD), in the pH range 4-7. The complex bound to the magnetic particles was released by treatment with a strong base, of which the recovery was 81.7%. As a reference, a solid phase extraction (SPE) column packed with Chelex-100 resin was employed for separation under similar conditions and produced comparable results. The tagging technique complemented polydimethylsiloxane (PDMS) microarray chip sampling in LA-ICP-MS, allowing determination of small sample volumes at high throughputs. For application, immunoglobulin G (IgG) was immobilized on the pillars of PDMS microarray chips and then tagged with the prepared Gd complex. IgG could then be determined through measurement of Gd by LA-ICP-MS. A detection limit of 1.61 ng/mL (${\pm}0.75%$ RSD) for Gd was obtained.

Evaluation of LA-ICP-MS Whole Rock Trace Element Analysis Using Fused Glass Bead of Silicate Rocks (규산염 암석의 알칼리 용융 유리원판에 대한 LA-ICP-MS 전암 미량원소 분석법 평가)

  • Kim, Myong Jung;Kim, Taehoon;Park, Kye-Hun;Lee, Ye Ji;Yang, Yun Seok;Moon, Jeongjin
    • The Journal of the Petrological Society of Korea
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    • v.24 no.2
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    • pp.141-147
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    • 2015
  • Using laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), we evaluated the reliability of trace element abundance data measured from the silicate rock references of JR-3, JG-3, JGb-1 and JB-1b using glass discs made by alkali fusion. For 28 elements including rare earth elements, relative standard deviations (RSD) are better than 7% in case when the concentrations of the elements in the rock samples are greater than 10 ppm. However, RSD shows somewhat increased values for the concentrations less than 10 ppm, but never exceeds 25%. Compared with previously reported averages of the compiled abundance data, our data display satisfactory results for the most cases with differences less than 10%. We suggest that LA-ICP-MS analysis using fused glass beads is a reliable, precise and time-saving method of trace element analysis for the silicate rocks spanning from mafic to felsic compositions.

Analytical Techniques Using ICP-MS for Clinical and Biological Analysis

  • Ko, Jungaa;Lim, H. B.
    • Mass Spectrometry Letters
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    • v.6 no.4
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    • pp.85-90
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    • 2015
  • This article reviews recent analytical techniques using inductively coupled plasma-mass spectrometry (ICP-MS) immunoassay for clinical and bio analysis. We classified the techniques into two categories, direct and indirect analysis, which depend upon a guideline of whether tagging materials are used or not. Direct analysis is well known, and generally used in conjunction with various other techniques, such as laser ablation, chromatographic separations, etc. Recently, indirect analysis using tagging elements has intensively been discussed because of its importance in future applications to bio and clinical analysis, including environmental and food industries. The method has shown advantages of multiplex detection, excellent sensitivity, and short analysis time owing to signal amplification and magnetic separation. Now, it expands the application field from small biomolecules to large cells.

Analysis of the Concentration of Metal Elements in Freshwater Fish Otolith Using LA-ICP/MS (LA-ICP/MS를 이용한 담수 어류 이석 내 금속 원소 농도 분석)

  • Park, Hyun Woo;Yoon, Suk-Hee;Park, Jaeseon;Lim, Bo-Ra;Lee, Hyeri;Choi, Jong Woo
    • Korean Journal of Ecology and Environment
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    • v.52 no.4
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    • pp.324-332
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    • 2019
  • In this study, the possibility of a follow-up study on environmental pollution in domestic freshwater was identified by analyzing fish otoliths using Laser ablation-inductively coupled mass spectrometry (LA-ICP/MS). Fish otolith are known to be affected by the environment in which fish live. As a result, research on this subject is active in many countries; however, this is not the case in Korea. Therefore, in this study, the possibility of tracing environmental pollution using fish otoliths was identified by analyzing the components of metal elements used as indicators for environmental pollution. For the component analysis of metallic elements LA-ICP/MS, which can shorten analysis time by reducing the pretreatment process, was used. Sampling was conducted by dividing the research and the background area and carp, a freshwater species, was selected as the experimental fish species subject. Based on the established LA-ICP/MS conditions, the concentration of the metallic elements in the fish otoliths collected in the research area was 2202.9 mg kg-1, 2.03 times higher than the 1,086.3 mg kg-1 in the background area. All elements except for Li and U, were found to be higher in the research area than in the background area. Compared with the sediment measuring net analysis data, the distribution tendency of Zn, Pb, and Cu in sediment metal element concentrations in the two regions and distribution of metal element concentration in fish otoliths were similarly shown. These results confirm that fish otoliths can be used to track environmental pollutants, such as in sediments.

Natural isotopes and trace element analyses in glass samples (판유리 시료에서 동위원소 및 미량원소 분석법)

  • Min, Ji-Sook;Heo, Sangcheol;Kim, Jae-Guin;Kim, Eun-Ho;Kim, Dong-Wook;Chung, Hee-Sun
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.219-226
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    • 2007
  • Glass is frequently encountered as types of materials that are submitted to forensic science laboratories as a result of trace evidence transfers. The repeatability and the reproducibility of trace element analysis were presented. An analysis of variance (ANOVA) was performed on laser ablation inductively coupled plasma spectrometric analyses of the fragments to identify the source. Pairwise comparisons were completed for all samples. In a pairwise comparison, each sample was compared to each other for a possible [n(n-1)/2] (n : numbers of the samples) total comparison to associate/discriminate samples using Tukey's HSD method. The aim of this study was to determine the utility of LA-ICP-MS for multi-element analysis of forensic samples. The 12 glass fragments from two manufacturers were collected and analyzed to identify the source. An analysis of variance (ANOVA) was performed on 31 elements in NIST 612 Trace elements in Glass. Elements were classified into four categories defined by the combination of precision and variation of inter-samples. We selected 11 elements, 209Bi, 90Zr, 121Sb, 178Hf, 59Co, 238U, 208Pb, 140Ce, 118Sn, 49Ti and 137Ba. 6 pairs out of 66 possible pairs were not distinguished when compared by 137Ba (p<0.05). However, all samples were distinguished using both 49Ti and 137Ba (p<0.05). In conclusion, multi-elemental analysis with LA-ICP-MS is a potential tecnique for the discrimination of forensic samples.