• Title/Summary/Keyword: 표준인증시료

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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).

Intercomparison and Determination of Trace Elements in Urban Dust by Neutron Activation Analysis (중성자방사화분석법을 이용한 대기분진중의 미량원소 비교분석)

  • Chung, Yong-Sam;Moon, Jong-Hwa;Kim, Sun-Ha;Park, Kwang-Won;Kang, Sang-Hun
    • Analytical Science and Technology
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    • v.13 no.2
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    • pp.179-188
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    • 2000
  • Trace elements in air samples artificially loaded on filters with urban dust and the bulk material of urban dust as an environmental sample were determined non-destructively using instrumental neutron activation analysis. Standard reference material (Urban Dust, SRM 1648) of the National Institute of Standard and Technology was used for the analytical quality control. The relative error for 37 elements was less than 15% and the standard deviation was less than 10%. 29 elements in the urban dust and 21 elements in the loaded filter sample were determined respectively. To evaluate the proficiency and reliability of the measurement, data intercomparison was performed and 39 analytical laboratories participated in the analysis using different analytical methods; neutron activation analysis, particle induced X-ray emission analysis, X-ray fluorescence analysis and atomic absorption spectrometry. Z-scores were calculated using the standard deviation of the laboratorie's mean as target standard deviation, and a good result was obtained that the values fall between -1 and +1 except some elements.

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Simultaneous Determination of Vitamin A and E in Infant Formula by Rapid Extraction and HPLC with Photodiode Array Detection (신속추출법 및 PDA-HPLC에 의한 조제분유 중 비타민 A, E의 동시분석)

  • Kwak, Byung-Man;Lee, Ki-Woong;Ahn, Jang-Hyuk;Kong, Un-Young
    • Korean Journal of Food Science and Technology
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    • v.36 no.2
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    • pp.189-195
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    • 2004
  • Rapid and simple method was developed for simultaneous determination of vitamins A and E contents in infant formula. Vitamins A and E were extracted by PDA-HPLC with reversed phase column using organic solvent, and their contents in Certified Reference Material (CRM) and infant formula were determined and compared with results of Food Standards Codex and AOAC method for evaluation of developed method, Vitamins A and E contents in CRM determined by developed method were within certified range of standard values. Developed method has great advantages of simple and rapid sample preparation and simultaneous determination of vitamins A and E by PDA-HPLC using reversed phase column.

Determination of trace boron in steels by prompt gamma-ray activation analysis (즉발감마선방사화분석법에 의한 철강시료 중의 붕소 측정)

  • Kim, I.J.;Cho, K.H.;Paul, R.L.
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.302-306
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    • 2009
  • A trace amount of boron in steel significantly influences its mechanical and physical properties. A prompt gamma ray activation analysis (PGAA) method is used to measure boron in low alloy steel samples of KRISS 101-01-C21~C26. NIST SRMs of 362, 364, 1761 and 1767 serve as the control standards to validate the measurement method. The measured values of the NIST SRMs are consistent with their certified values within the expected uncertainties, except for that of NIST SRM 362. Experimental uncertainties are evaluated according to the guidelines given by the International Organization for Standardization (ISO). The expanded uncertainties are calculated with a coverage factor of 2, at approximately 95% confidence level. The calculated relative expanded uncertainties of boron mass fractions are between 3% and 7% at the mg/kg level. The results are compared with the results measured by the solvent extraction-inductively coupled optical emission spectrometry (ICP/OES) method.

Preparation of wastewater-based reference materials for heavy metal analysis and interlaboratory study (중금속분석용 폐수표준물질 제조 및 실험실간 비교평가)

  • Kim, Young-Hee;Song, Ki-Bong;Shin, Sun-Kyoung;Lee, Jung-Sub;Jeong, Gi-Taeg;Hong, Eun-Jin;Park, Jin-Ju;Yu, Suk-Min
    • Analytical Science and Technology
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    • v.23 no.3
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    • pp.295-303
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    • 2010
  • In this study, the wastewater-based reference material (RM) was prepared and certified for 7 trace metal elements with evaluation of uncertainties. The RM was distributed to 25 laboratories for the interlaboratory comparison testing. The certified values and expanded uncertainties were derived using ISO guideline 35 and the standard uncertainties for homogenieties were 0.43~2.67% of certified values. The analytical results from the interlaboratory comparison testing showed normal distributions and the robust means from the interlaboratory comparison testing were higher than the certified values of the RM for all analytes.

Multi - elemental Analysis of Hair by Inductively Coupled Plasma/Mass Spectrometry (유도결합 플라스마 질량분석법에 의한 모발의 다원소 분석)

  • Cha, Myung Jin;Kang, Jun Mo;Park, Chang Joon
    • Analytical Science and Technology
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    • v.15 no.4
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    • pp.335-340
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    • 2002
  • An analytical method has been developed to determine multi-elements in human hair samples by inductively coupled plasma mass spectrometry (ICP-MS). 0.05 g of hair sample was added to the Teflon digestion bomb together with 1.5 mL of nitric acid and an appropriate amount of In as an internal standard. The sample was then decomposed in the microwave digestion system. The hair certified reference material, GBW 09101, was analyzed for the validation of the analytical method. The determined values were in good agreement with the certified values within the uncertainty range.

A Comparative Study on the Determination of the Selenium in Biological Samples using 75Se and 77mSe Nuclides (75Se과 77mSe 핵종을 이용한 생물시료 중의 셀렌 분석에 대한 비교 연구)

  • Moon, Jong-Hwa;Kang, Sang-Hoon;Kim, Sun-Ha;Chung, Yong-Sam;Kim, Young-Jin
    • Analytical Science and Technology
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    • v.18 no.1
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    • pp.23-26
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    • 2005
  • Se is well known as an anti-oxidant trace element and many customers are interested in an analysis and contents of Se in the various foodstuff samples. This study was aimed at establishig and comparing an analytical method for the determination of the Se in biological samples by neutron activation analysis using two nuclides, $^{75}Se$ and $^{77m}Se$. Keeping this objective, three NIST biological standard reference materials were chosen and the concentrations of the Se were determined under the prefixed analytical conditions such as the irradiation, decay and measurement time. The measured values by both analytical methods were evaluated with certified values. In addition, the detection limits and measurement uncertainty for the analytical results using $^{75}Se$ and $^{77m}Se$ were compared with each other.

Simultaneous Determination of Vitamin $D_3\;and\;K_1$ in Infant Formula by Column-switching High Performance Liquid Chromatography with UV Detection (Column-switching HPLC를 이용한 성장기용 조제식 중 비타민 $D_3,\;K_1$의 동시분석)

  • Kwak, Byung-Man;Ahn, Jang-Hyuk;Chang, Chi-Hoon
    • Korean Journal of Food Science and Technology
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    • v.37 no.6
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    • pp.1024-1027
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    • 2005
  • Rapid and simple method was developed for simultaneous determination of vitamins $D_3\;and\;K_1$ contents in infant formula. Contents of vitamins $D_3\;and\;K_1$, extracted by column-switching HPLC with reversed phase column using enzymatic hydrolysis and organic solvent, in CRM determined by developed method were within certified ranges of standard values.

Comparison of the Heavy Metal Analysis in Soil Samples by Bench-Top ED-XRF and Field-Portable XRF (Bench-Top ED-XRF 및 휴대용 XRF를 이용한 토양 시료 중의 중금속 비교 분석)

  • Choi, Soo-Jung;Kim, Chong-Hyeak;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.293-301
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    • 2009
  • As a basic research for development of the domestic field-portable XRF spectrometer, we discussed the analytical results of bench-top ED-XRF and field-portable XRF method for polluted heavy metals such as Cr, As, Se, Hg, Pb, Cd in soil samples. To obtain the best performance of the XRF spectrometer, the instrumental parameters of X-ray tube-voltage and measurement time were optimized for 6 heavy-metal elements in soil using certified reference material. The quantitative analysis of Cr, As, Se, Hg, Pb, Cd concentration in certified reference materials and soil samples were compared by empirical method and fundamental parameter method.

Comparison study of the wear metal analysis in oil sample by portable and bench-top XRF (휴대용 및 Bench-Top X-선 형광 분석기를 이용한 오일 시료 중 마찰 금속의 비교 분석)

  • Choi, Soo-Jung;Kim, Chong-Hyeak;Lee, Sueg-Geun;Kim, Dong-Pyo
    • Analytical Science and Technology
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    • v.22 no.5
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    • pp.422-431
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    • 2009
  • The analytical results of wear metals such as Na, Mg, Al, Si, P, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Mo, Ag, Cd, Sn, Ba, Pb in oil samples are compared by portable and bench-top XRF methods as a basic study for the development of portable X-ray fluorescence spectrometer. The instrumental parameters such as measurement time of portable and bench-top XRF were optimized using certified reference materials of hydrocarbon oil with 20 wear metals in concentration range from 10 to 900 mg/kg. The analytical results of 20 wear metals in certified reference materials and new/used engine oil samples were compared by empirical and fundamental parameter methods.