• Title/Summary/Keyword: CRM (certified reference material)

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The Evaluation of Proficiency Test between Radioimmunoassay and Chemiluminescence Immunoassay (방사면역측정법과 화학발광면역측정법간의 숙련도 비교평가)

  • Noh, Gyeong-Woon;Kim, Tae-Hoon;Kim, Ji-Young;Kim, Hyun-Joo;Lee, Ho-Young;Choi, Joon-Young;Lee, Byoeng-Il;Choe, Jae-Gol;Lee, Dong-Soo
    • The Korean Journal of Nuclear Medicine Technology
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    • v.15 no.2
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    • pp.116-124
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    • 2011
  • Purpose: To establish accurate external quality assurance (EQA) test, cross institutional and modality tests were performed using WHO certificated reference material (CRM) and same pooled patients serum. Materials and Methods: Accuracy and precision were evaluated using CRM and pooled patients' serum for AFP, CEA, PSA, CA 125, CA 19-9, T3, T4, Tg, TSH. To evaluate the accuracy and precision, recover test and coefficient variation were measured. RIA test were performed in major 5 RIA laboratory and EIA (CLIA) test were done in 5 major EIA laboratory. same sample of CRM and pooled serum were delivered to each laboratory. Results: In 2009, mean precision of total tumor marker of RIA was $14.8{\pm}4.2%$ and that of EIA(CLIA) was $19.2{\pm}6.9%$. In 2010, mean precision of 5 tumor marker and T3, T4, Tg, TSH was $13.8{\pm}6.1%$ in RIA and $15.5{\pm}7.7%$ in EIA (CLIA). There was no significant difference between RIA and EIA. In RIA, the coefficient variations (CV) of AFP, CEA, PSA, CA 125, T3, T4, TSH were within 20%. The CV of CA 19-9 was over 20% but there was no significant difference with EIA (CLIA) (p=0.345). In recovery test using CRM, AFP, PSA, T4, TSH showed 92~103% of recovery in RIA. In recovery test using commercial material, CEA, CA 125, CA 19-9 showed relatively lower recovery than CRM but there was no significant difference between RIA and EIA (CLIA). Conclusion: By evaluating the precision and accuracy of each test, EQA test could more accurately measured the quality of each test and performance of laboratory.

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Determination of $^{226}Ra$ Isotope in the Leachate around Phosphogypsum Stack Using Ethylenediaminetetraacetic Acid (EDTA) (Ethylenediaminetetraacetic acid (EDTA)를 이용한 인산석고 야적장 침출수 중의 $^{226}Ra$ 분석법 개발)

  • Kim, Geun-Ho;Kim, Yong-Jae;Chang, Byung-Uck
    • Journal of Radiation Protection and Research
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    • v.36 no.4
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    • pp.223-229
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    • 2011
  • Ba is the most useful element to get the $Ba(Ra)SO_4$ precipitate. However, when the high concentrations of ions such as sulfate, calcium are existed in the leachate of phosphogypsum stack, it is difficult to get the $Ba(Ra)SO_4$ precipitate. Since this reason, the developed method for the Ba coprecipitate using EDTA was performed to determine the $^{226}Ra$ concentration in the high sulfate sample. The average concentration of $^{226}Ra$ in a leachate of phosphogypsum using this method was 0.102 $Bq{\cdot}kg^{-1}$ and the minimal detectable activity is 3.4 $mBq{\cdot}kg^{-1}$. The $mBq{\cdot}kg^{-1}$ method was 0.102 $Bq{\cdot}kg^{-1}$ and the minimal detectable activity is 3.4 $mBq{\cdot}kg^{-1}$. The $^{226}Ra$ stock solution and the CRM (Certified Reference Material) were analyzed to verify this method. In analyzed $^{226}Ra$ stock solution, bias with added concentration was approximately 1% and the correlation curve between $^{226}Ra$ concentration in simulated standard sample and measured $^{226}Ra$ concentration showed good agreement with a correlation coefficient ($R^2$) of 0.99. In analyzed CRM, maximum bias with reference value was 5.8% (k=1) and the analytical results were in good agreement with the reference value.

Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

  • Yim, Yong-Hyeon;Park, Ji-Youn;Han, Myung-Sub;Park, Mi-Kyung;Kim, Byung-Joo;Lim, Young-Ran;Hwang, Eui-Jin;So, Hun-Young
    • Bulletin of the Korean Chemical Society
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    • v.26 no.3
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    • pp.440-446
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    • 2005
  • A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

Determination of trace arsenic in seawater by flow injection-hydride generation inductively coupled plasma mass spectrometry (연속흐름주입-수소화물생성-유도결합플라스마 질량분석장치를 이용한 바닷물표준시료중의 극미량 비소분석방법의 확립)

  • Suh, Jung-Ki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.316-325
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    • 2008
  • An inductively coupled plasma mass spectrometry (ICP-MS) instrument equipped with flow injection-hydride generation system was used for the determination of trace arsenic in seawater sample. The accuracy in this method was verified by the analysis of certified reference materials (CRM) of seawater (CASS-4, NASS-5). The analytical results agreed with certified value within the range of uncertainty. The expanded uncertainties for CASS-4 and NASS-5 in this experiment were ranged from 6.2% to 6.8% obtained from repeated analyses of the CRMs (n=5). The detection limit of $As^+$ (m/z=74.9216) in this method was confirmed about 0.01 ug/kg. Linearity obtained from calibration curve of arsenic was excellent ($R^2=1$). The detection at $As^+$ (m/z=74.9216) and $AsO^+$ (m/z=90.9165) by using oxygen reaction gas in DRC mode was compared. Sensitivity at $AsO^+$ (m/z=90.9165) was decreased about 25-fold, but the analytical results are the same that at $As^+$ (m/z=74.9216).

The Study on Analysis Method and Performance Evaluation of Portable GC/MS (휴대용 GC/MS 성능검사 및 분석방법 연구)

  • Park, Yuonshin;Noh, Hyeran;Yang, Heeseon;Seok, Gwanseol
    • Journal of the Society of Disaster Information
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    • v.9 no.3
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    • pp.249-258
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    • 2013
  • Recieved Mar. 06, 2013 Revised Mar. 29, 2013 Accepted Sep. 11, 2013In this study, we evaluated the method performance and the optimum sample injection method of the portable GC/MS(HAPSITE) which were designed to operate on scene of chemical accidents. Chemicals used for performance test were vinyl chloride(VC), methyl chloride(MC), benzene(Bz), toluene(Tol). CRM(Certified Reference Material) Manufactured by KRISS(Korea Research Institute of Standards and Science) was used as the standard gas. The results showed that 1) Among three sample injection methods(Cylinder, Silico canister, and Bag), bag was identified as the most appropriate sample injection method. Bag material and capacity did not significantly affect the results. The most ideal reproducibility occurred at the 2-minute point of the purge time in the loop and tenax methods. 2) Performance evaluation of HAPSITE was conducted. Evaluation items were reproducibility, linearity, method detection limit, etc. Tenax concentration method was appropriate for larger molecules and Carbopack concentration method was suitable for smaller molecules.

Quantifying Uncertainty of Vitamin C Determination in Infant Formula by Indophenol Titration Method (인도페놀 적정법에 의한 성장기용조제식 중 비타민 C 함량분석의 측정불확도 산정)

  • Jun, Jang-Young;Kwak, Byung-Man;Ahn, Jang-Hyuk;Kong, Un-Young
    • Korean Journal of Food Science and Technology
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    • v.37 no.3
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    • pp.352-359
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    • 2005
  • Uncertainty involved during determination of vitamin C content in infant formula was quantified by indophenol titration method. Uncertainty sources in measurand, such as purity, weight, final volume of standard, volume of standard solution used for titration, sample weight, final volume of sample, extraction solution used for titration, titration of extraction solution and standard solution by indophenol solution were identified and used as parameters for combined standard uncertainty based on Guide to the expression of uncertainty in measurement (GUM) and Draft EURACHEM/CITAC Guide. Uncertainty parameters of each source in measurand were identified as resolution, reproducibility and stability of chemical balance, standard material purity, repeatability, reproducibility, end point of titration, 1 mL pipet, 5 mL autopipet, and 100 mL mass flask. Each uncertainty component was evaluated by types A and B and included to calculate combined uncertainty. Analytical test result for traceability under laboratorial conditions using Certified Reference Material (CRM) test was certified as $108.4{\pm}1.7mg/100g$, which was within CRM certification range of $114.6{\pm}6.6mg/100g$. Uncertainty test result of vitamin C content of 5 g sampling was $56.7{\pm}2.44mg/100g$. Uncertainty could be reduced by identification of uncertainty sources and components related with vitamin C determination by indophenol titration method and by decreasing uncertainty sources and components.

Contents of Heavy Metals in Fishes from the Korean Coasts (한국 연안산 어류의 중금속 함량)

  • Mok, Jong-Soo;Shim, Kil-Bo;Cho, Mi-Ra;Lee, Tae-Seek;Kim, Ji-Hoe
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.4
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    • pp.517-524
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    • 2009
  • We collected 177 fishes representing 53 species of fish from the eastern (Pohang), western (Gunsan), and southern (Tongyeong) coasts of Korea, and measured their heavy metal contents. The mean recoveries of the heavy metals extracted from cod muscle (certified reference material, CRM) were $88.7{\sim}100.6%$. The mean levels of the heavy metals in the samples taken from the edible portion of each fish were high in the order of Zn ($8.981{\pm}4.835{\mu}g/g$), Cu ($0.755{\pm}0.507{\mu}g/g$), and Mn ($0.433{\pm}0.699{\mu}g/g$), which are necessary metals in the human body, and then followed by Cr ($0.206{\pm}0.181{\mu}g/g$), Ni ($0.081{\pm}0.110{\mu}g/g$), Pb ($0.038{\pm}0.046{\mu}g/g$), Cd ($0.017{\pm}0.023{\mu}g/g$). The average daily intakes of the heavy metals by the fishes were as follows: Cd (0.81 ${\mu}g$), Cr (9.98 ${\mu}g$), Cu (36.63 ${\mu}g$), Mn (21.01 ${\mu}g$), Ni (3.93 ${\mu}g$), Pb (1.84 ${\mu}g$) and Zn (435.58 ${\mu}g$). The average weekly intakes of Cd, Cu, Pb and Zn by the fishes were 1.35%, 0.12%, 0.86%, and 0.73% respectively, as compared with PTWI (Provisional Tolerable Weekly Intakes) established by FAO/WHO Expert Committee for Food Safety Evaluation.

Determination of halogen elements in plastics by using combustion ion chromatography (연소IC를 이용한 플라스틱 중 할로겐 물질 정량)

  • Jung, Jae Hak;Kim, Hyo Kyoung;Lee, Yang Hyoung;Lee, Lim Soo;Shin, Jong Keun;Lee, Sang Hak
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.284-295
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    • 2008
  • For plastics samples, a method using combustion ion chromatography was selected as a method for rapid low-cost analysis to test whether hazardous substances are contained or not. Using combustion ion chromatography, a verification test for F, Cl and Br compounds generated a linear calibration curve with a correlation coefficient of $r^2$ = 0.999~1.000 in the calibration range from 0.5 to 4.0 mg/kg. The detection limits were found to be 0.005~0.024 mg/kg and quantitative limits were found to be 0.014~0.073 mg/kg. The recoveries of combustion ion chromatography using certified reference material (CRM) were found to be 95.5~104.9%. Based on these results, a proficiency test was conducted together with several laboratories in and out of the country, to make comparative analysis of the results from each laboratory. As a result, the data supported the use of combustion ion chromatography as an effective analysis method to deal with regulations for halogen-free electronic products and for other hazardous substances in the electronic products.

A Study on Trace-metals in Korean Yeongdeok Crab and Russian Snow Crab (영덕대게와 러시아산대게의 체내 미량금속 함량 연구)

  • Kim, Cho-Ryeon;Yoon, Yi-Yong
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.14 no.3
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    • pp.147-153
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    • 2011
  • This study is to measure the differences of the trace-metals resulted from the different ecologies, such as nickel(Ni), copper(Cu), zinc(Zn), cadmium(Cd), plumbum(Pb), arsenic(As) and chrome(Cr) remaining in the parts of Korean Yeongdeok Crab (KYC) and Russian Snow Crab (RSC) based on ICP-MS. The recovery rate of each metal certified the reference materials (CRM) was in the average of 81~99%, which corresponded with the level required in Codex. The level of metals in the parts of KYC was in the order of Ni > As > Zn > Cu > Cr > Cd in the both male and female shell; the order of Zn > As > Cu > Cr > Ni > Cd in the leg flesh; the order of Zn > As > Cu > Cr > Cd > Ni in the body flesh; the order of Cu > Zn > As > Cd > Cr > Ni in the gill; the order of Cu > As > Zn > Cd > Ni > Cr in the male hepatopancreas; the order of Cu > Zn > As > Cd > Cr > Ni in the female hepatopancreas, thereby showing some differences. It was revealed that the levels of most metals (nickel, copper, zinc, arsenic and chrome) were similar between KYC and RSC except cadmium which was somewhat lower than that of KYC. However, the cadmium in RSC was discovered in high level in most of the parts, two times higher in the hepatopancreas, and four times in the gill. It was also revealed that the trace metal contents were changing according to the size of KYC; the metals with the highest level of Ni in shell, Zn in leg and body flesh, Cu in gill tended to decrease as growing, whereas the cadmium contents tended to increase overall and accumulated the most in hepatopancreas. The results showed there was a possibility that the phenomenon of bioaccumulation within hepatopancreas would increase as growing.

A Study on the Self-absorption Correction Method of HPGe Gamma Spectrocopy Analysis System Using Check Source (Check Source를 이용한 HPGe감마핵종분석시스템의 자체흡수 보정방법 연구)

  • Jeong-Soo, Park;Hyo-Jin, Lim;Hyun-Soo, Seo;Da-bin, Jang;Myoung-Joon, Kim;Sang-Bok, Lee;Sung-Min, Ahn
    • Journal of radiological science and technology
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    • v.45 no.6
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    • pp.523-529
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    • 2022
  • Gamma spectroscopy analysis is widely used for radioactivity analysis, and various factors are required for radioactivity calculations. Among the factors, K3 for each sample significantly influences the results. The previous methods of correcting the self-absorption effect include a computational simulation method and a method that requires making a CRM(certified reference material) identical to the sample medium. However, the above methods have limitations when used in small institutions because they require specialized program utilization skills or high manufacturing costs and large facilities. The aim of this study is to develop a method that can be easily and rapidly applied to radioactivity analysis. After filling the beaker with water, we placed the radiation source in a uniform position and used the measured value as the benchmark. Next, a correction factor was derived based on the difference in the radiation source count of the benchmark and the identically measured sample. For the radiation source, Eu-152, which emits a broad range of energy within the measurement range of gamma rays, and Cs-134 and Cs-137, which are indicator nuclides in environmental radiation analysis, were used. The sample was selected within the density range of 0.26-2.11 g/cm3, and the correction factor was derived by calculating the count difference of each sample compared to the reference value of water. This study presents a faster and more convenient method than the existing research methods for determining the self-absorption effect correction, which has become increasingly necessary.