• Title/Summary/Keyword: isotope measurement

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Accurate Determination of Malachite Green and Leucomalachite Green in Fish using Isotope Dilution Liquid Chromatography/Mass Spectrometry (ID-LC/MS)

  • Ahn, Seong-Hee;Kim, Byung-Joo;Lee, Yun-Jung;Kim, Jeong-Kwon
    • Bulletin of the Korean Chemical Society
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    • v.31 no.11
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    • pp.3228-3232
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    • 2010
  • Malachite green (MG) has been used world-widely in aquaculture as a parasiticide or fungicide. Although MG performed successfully, it has not been permitted for use in aquaculture from European Union, USA, and Canada because of its carcinogenicity and mutagenicity. We developed a sensitive and specific method to determine MG and its principal metabolite, leucomalachite green (LMG), respectively by isotope dilution liquid chromatography mass spectrometry (ID-LC/MS). To enhance the extraction recovery of MG and LMG from fish tissue, an additional step, saponification, was introduced in sample preparation process to remove fat in sample extract, which hampered the performance of SPE columns. The residue of MG and LMG in fish was analyzed using liquid chromatography mass spectrometry in the selected ion monitoring (SIM) mode by monitoring at m/z 329 and 334 for MG and $d_5$-MG and at m/z 331 and 337 for LMG and $^{13}C_6$-LMG, respectively. This method was validated by comparing with the value of the reference material provided by Laboratory Government Chemistry (LGC). The results agreed within the measurement uncertainty and the accuracy was much improved than the provided reference value by LGC.

Evaluation of Organic Matter Sources of Phytoplankton in Paldang Reservoir using Stable Isotope Analysis (팔당호 내 식물플랑크톤 안정동위원소 분석을 통한 유기물 기원 평가)

  • Kim, Jongmin;Kim, Bokyong;Kim, Minseob;Shin, Kisik
    • Journal of Korean Society on Water Environment
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    • v.31 no.2
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    • pp.159-165
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    • 2015
  • The organic matter sources of phytoplankton and related environmental factors influencing algal bloom in Paldang reservoir were studied using nitrogen and carbon isotope ratio(${\delta}^{15}N$, ${\delta}^{13}C$). Phytoplankton samples for stable isotope analysis were collected from four points in reservoir using a plankton net. Physicochemical water quality, algal taxa and hydrological data were collected from published monitoring material. Phytoplankton samples were analyzed by IRMS. CN ratio of each sample was very similar to that of phytoplankton from literature cited. ${\delta}^{15}N$ of each sample was decreased during July. Mixing and dilution of nitrogen sources due to increment of influx by concentrated rainfall were considered as the main reason for the decline of ${\delta}^{15}N$. Based on analyzed ${\delta}^{15}N$ value of each sample, nitrogen source of Bughan river sample was presumed to come from soil. The nitrogen sources of Namhan river and Kyeongan stream samples seemed to be sewage or animal waste. Low ${\delta}^{15}N$ value in August (2012) seemed to be influenced by isotope fractionation due to the blooming of nitrogen-fixation blue-green algae (Anabaena spp.). Variation in ${\delta}^{15}N$ values particularly by blue-green algal bloom was considered the important factor for estimating the organic matter sources of phytoplankton.

Inter-laboratory Comparison of Stable Carbon and Nitrogen Isotopic Composition Data Using Elemental Analyzer-isotope Ratio Mass Spectrometers

  • Kim, Jung-Hyun;Kang, Sujin;Bong, Yeon-Sik;Park, Kwangkyu;Kang, Tae-Woo;Park, Yong-Se;Kim, Dahae;Choi, Seunghyun;Joo, Young Ji;Choi, Bohyung;Nam, Seung-Il;Lee, Sang-Mo;Shin, Kyung-Hoon
    • Journal of Environmental Analysis, Health and Toxicology
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    • v.21 no.4
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    • pp.229-236
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    • 2018
  • In this study, inter-laboratory comparison was done using elemental analyzer-isotope ratio mass spectrometers (EA-IRMSs) to determine carbon and nitrogen contents as well as stable carbon and nitrogen isotopic compositions (${\delta}^{13}C$ and ${\delta}^{15}N$) of five environmental samples containing lake and marine sediments, higher plant leaves, and fish muscle, and one organic analytical standard (Protein (Casein) Standard OAS). Five national laboratories participated in this comparison study, and each laboratory analyzed all five samples and the analytical standard. Results showed that variations in total organic carbon (TOC) and total nitrogen (TN) contents as well as ${\delta}^{13}C_{TOC}$ and ${\delta}^{15}N_{TN}$ values among the laboratories were large compared to the analytical uncertainties. The results highlighted the inhomogeneity of the test samples and thus, the need to select suitable standard reference materials for future inter-laboratory studies. Further inter-laboratory comparison exercises could promote good measurement practices in the acquisition of stable carbon and nitrogen isotopic composition data.

METHODOLOGICAL ASPECTS OF THE IN VIVO MEASUREMENT OF ILEAL AMINO ACID DIGESTIBILITY IN PIGS - A REVIEW -

  • Yin, Y.-L.;McGracken, Kelvin J.
    • Asian-Australasian Journal of Animal Sciences
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    • v.9 no.5
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    • pp.495-502
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    • 1996
  • Much recent research on protein and amino acid (AA) digestive physiology of pigs has been concerned with measurement of the ileal apparent and true digestion and absorption. For measurement of the ileal apparent digestibility of AA, the steered ileo-caecal valve cannulation (SICV) and the ileo-rectal anastomosis (IRA) techniques appear to be the more reliable and simple methods, when compared with any methods requiring use of a marker for calculation of digestibility, or with the complex techniques of ileo-caecal re-entrant cannula (ICRC) and the postvalve ileo-colic re-entrant cannula (IPVC). On the other hand, the peptide alimentation ultrafiltration methods might be a better choice for measurement of the ileal endogenous nitrogen (N) and AA flow in a routine feedstuff analysis, although the classical method of $^{15}N-isotope$ dilution method is still a standard method for N and AA nutrition research in pigs.

Stable Isotope Measurement of Ammonium Using HPLC-RTS (high performance liquid chromatography-retention time shift) (HPLC-RTS (high performance liquid chromatography-retention time shift)를 이용한 암모늄 이온의 안정동위원소 측정방법의 개선)

  • An, Soonmo;Lee, Jiyoung;Gardner, Wayne S.
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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    • v.18 no.1
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    • pp.47-52
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    • 2013
  • Despite the usefulness of nitrogen isotope tracer experiments in nitrogen cycling studies, there are not such many measurement data mainly due to the difficulties in analytical methods. Although Gardner et al. (1996) developed a relatively simple and accurate method that can measure ammonium isotope using HPLC and used it widely in various N dynamics studies, the technique was not adopted to other laboratories. An HPLC-RTS system using updated HPLC pumps that can perform the same measurements as that of Gardner et al. (1996) was built. The result of standard sample showed linear increase of RTS with the $^{15}N$ proportions. Centroid retention times calculated with Matlab$^{(R)}$ program enhanced the linearity of the response. In a sea water incubation experiment spiked with $^{15}NH_4{^+}$, the uptake and regeneration of ammonium could be separately estimated using the temporal change of $^{15}N/^{14}N$.

A Comparative Study of Branching Ratio of 167Yb Radioactive Isotope from Gamma-ray Spectrum Produced by 169Tm(p,3n)167Yb Reaction with 100-MeV Proton Beam (100-MeV 양성자 빔을 이용하여 169Tm(p,3n)167Yb 반응에 의해 생성된 167Yb 방사성동위원소에서 방출되는 감마선 스펙트럼 비교 연구)

  • Sam-Yol, Lee
    • Journal of the Korean Society of Radiology
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    • v.16 no.7
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    • pp.953-960
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    • 2022
  • The measurement of branching ratio of 167Yb radioactive isotopes from gamma-ray spectrum of 169Tm(p,3n)167Yb reaction were performed by using a 100-MeV proton linear accelerator of the Korea Multi-purpose Accelerator Complex (KOMAC). The 167Yb isotope has a half-life of 17.5 minutes and decays to 169Tm. The gamma rays generated from the 167Yb isotope were measured using an HPGe detector gamma ray spectroscopy system. The energy calibration of the detector and the efficiency measurement of the detector were determined using a standard source. The gamma rays of known main energy (62.9, 106.2, 113.3, 143.5 and 176.3 keV) were measured. On the other hand, information about the intensity of the generated gamma rays is very inaccurate. Therefore, in this study, the decay strength of the main gamma rays was accurately measured. Overall, it was different from the previously known results, and in particular, it was found that the intensity of the main decay gamma ray, such as the 113.3 and 106.2 keV gamma ray, was overestimated, and it was found that the gamma ray, such as 62.9, 116.7 and 143.5 keV was underestimated. The present results are considered to be important information in the fields of nuclear fusion, astrophysics and nuclear physics in the future.

Automated Cold Volume Calibration of Temperature Variation in Cryogenic Hydrogen Isotope Sorption Isotherm (극저온(20K) 수소동위원소 흡착 등온선의 온도 변화에 대한 자동 저온 부피 교정)

  • Park, Jawoo;Oh, Hyunchul
    • Korean Journal of Materials Research
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    • v.29 no.5
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    • pp.336-341
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    • 2019
  • The gas adsorption isotherm requires accurate measurement for the analysis of porous materials and is used as an index of surface area, pore distribution, and adsorption amount of gas. Basically, adsorption isotherms of porous materials are measured conventionally at 77K and 87K using liquid nitrogen and liquid argon. The cold volume calibration in this conventional method is done simply by splitting a sample cell into two zones (cold and warm volumes) by controlling the level sensor in a Dewar filled with liquid nitrogen or argon. As a result, BET measurement for textural properties is mainly limited to liquefied gases (i.e. $N_2$ or Ar) at atmospheric pressure. In order to independently investigate other gases (e.g. hydrogen isotopes) at cryogenic temperature, a novel temperature control system in the sample cell is required, and consequently cold volume calibration at various temperatures becomes more important. In this study, a cryocooler system is installed in a commercially available BET device to control the sample cell temperature, and the automated cold volume calibration method of temperature variation is introduced. This developed calibration method presents a reliable and reproducible method of cryogenic measurement for hydrogen isotope separation in porous materials, and also provides large flexibility for evaluating various other gases at various temperature.

Long term activity measurement of the primary circuit water on the LVR-15 research reactor

  • Ladislav Viererbl;Vit Klupak;Hana Assmann Vratislavska
    • Nuclear Engineering and Technology
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    • v.56 no.4
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    • pp.1250-1253
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    • 2024
  • Activity measurement of the primary circuit water of fission reactors is one method that can provide early detection of a damaged fuel assembly in the reactor core. This is an important aspect in the safe operation of the reactor and for radiation protection of staff. Radionuclides in the primary circuit water are produced by the activation of stable nuclides and the fission of fissile nuclides, mainly the isotope 235U. In the LVR-15 research reactor, measurement of the activity of the primary circuit water has been regularly undertaken since 1996. A water sample is taken from the primary circuit every week and the activities are measured four days later using gamma spectrometry. The results of these long-term measurements from 1996 to 2022 are presented. The activity time dependences of the individual radionuclides are discussed in relation to fuel assembly damage and for events connected to contamination of the water by objects inserted into the primary circuit during experiments carried out near the reactor core.

Accurate determination of chloramphenicol in meat by isotope dilution liquid chromatography mass spectrometry (ID-LC/MS) (동위원소희석 액체크로마토그래피-질량분석법을 이용한 육류 중 클로람페니콜의 정밀한 정량 분석에 관한 연구)

  • Song, Hye-Min;Kim, Byung-Joo;Jeong, Hyuk;Ahn, Seong-Hee
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.524-530
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    • 2010
  • Chloramphenicol is one of the most effective antibiotics for treatment of food-producing animals for typhoid fever. However, it has been reported that it caused severe side effects such as aplastic anemia in human, therefore the use of chloramphenicol for food-producing animal is prohibited by European Union and other countries. In this study, the analytical method using isotope dilution liquid chromatography-mass spectrometry (ID-LC/MS) was established for accurate determination of chloramphenicol in meat. Chloramphenicol was extracted with ethylacetate from porcine and solid phase extraction cartridge was used for enhancing the recovery. The residue of chloramphenicol in porcine was analyzed using the liquid chromatography mass spectrometer (LC/MS) interfaced with electrospray ionization source. Analysis was performed in negative mode with selected reaction mornitoring mode at m/z 321${\rightarrow}$257 of $[M-H]^-$ ${\rightarrow}$ $[M-H-(HCOCl)]^-$ and m/z 326 ${\rightarrow}$ 262 channels for its isotope. The established method was tested using fortified samples at the level of 0.2 1, 10, $25\;{\mu}g$/kg and analytical results agreed with the gravimetrically fortified values within their uncertainties. This method was validated by analyzing a certified reference material, BCR 445, from IRMM (Institute for Reference Materials and Measurement). Our measurement values agreed with the certified value within their uncertainties. The uncertainty of our measured value was much lower than that the certified value from IRMM.