• Title/Summary/Keyword: Metrology

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Measurement uncertainty for QC/QA applied to the chemical analysis (화학 분석 결과의 QA/QC를 위한 측정 불확도)

  • Woo, Jin-Chun;Oh, Sang-Hyub;Kim, Byoung-Moon;Bae, Hyun-Kil;Kim, Kwang-Sub;Kim, Young-Doo
    • Analytical Science and Technology
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    • v.18 no.6
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    • pp.475-482
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    • 2005
  • The expression of uncertainty applied to the chemical analysis is highly recommended with increasing demands upon the systematic quality assurance and control(QA/QC) with ISO 17025. For the quantification of quality source, 7 major common sources of uncertainty, normally contributing to the quality of the chemical analysis, were selected from QA/QC literatures of chemical analysis. They were classified into repeatability, drift, uncertainty in standards, linearity of calibration, homogeneity, stability of sample, and matrix effect. And, the quantification of the sources by means of measurement uncertainty was proposed as a prerequisite steps for QA/QC. Examples applied to the quantification procedures of modelling, combination and expression of standard uncertainty for the 7 major common sources were presented as a reference guide for QA/QC in chemical analysis.

Outlier Detection Method for Time Synchronization

  • Lee, Young Kyu;Yang, Sung-hoon;Lee, Ho Seong;Lee, Jong Koo;Lee, Joon Hyo;Hwang, Sang-wook
    • Journal of Positioning, Navigation, and Timing
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    • v.9 no.4
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    • pp.397-403
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    • 2020
  • In order to synchronize a remote system time to the reference time like Coordinated Universal Time (UTC), it is required to compare the time difference between the two clocks. The time comparison data may have some outliers and the time synchronization performance can be significantly degraded if the outliers are not removed. Therefore, it is required to employ an effective outlier detection algorithm for keeping high accurate system time. In this paper, an outlier detection method is presented for the time difference data of GNSS time transfer receivers. The time difference data between the system time and the GNSS usually have slopes because the remote system clock is under free running until synchronized to the reference clock time. For investigating the outlier detection performance of the proposed algorithm, simulations are performed by using the time difference data of a GNSS time transfer receiver corrected to a free running Cesium clock with intentionally inserted outliers. From the simulation, it is investigated that the proposed algorithm can effectively detect the inserted outliers while conventional methods such as modified Z-score and adjusted boxplot cannot. Furthermore, it is also observed that the synchronization performance can be degraded to more than 15% with 20 outliers compared to that of original data without outliers.

Development of certified reference materials for odorous aldehyde (알데하이드 악취물질의 인증표준물질 개발)

  • Kim, Young-Doo;Woo, Jin-Chun;Bae, Hyun-Kil;Kim, Byoung-Moon;Lee, Byung Gil;Heo, Gwi Suk
    • Analytical Science and Technology
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    • v.21 no.1
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    • pp.14-19
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    • 2008
  • Among the many odor materials, aldehyde has bad influences not only on human nose, but also on human health. Aldehyde has a strong odor at infinitesimal level, such as down to ppt concentration. Also aldehydes are highly reactive and have poor stability. Therefore, manufacture of standard gases, analysis of aldehydes are very difficult compare to other air pollution analysis. Aldehyde CRM containing 4 different aldehydes at $10{\mu}mol/mol$ (ppm) is developed by using gravimetry method according to ISO 6142 guide. The standard gases were reproduced again, and examined its reproducibility of preparation by GC-FID. The developed aldehyde CRM's certified value showed a relative expanded uncertainties of 2.11 % (95 % of confidence level, k=2).

Comparison of QuEChERS and Solid Phase Extraction for Accurate Determination of Pesticide Residues in Kimchi Cabbage and Strawberry using Isotope Dilution Mass Spectrometry

  • Seonghee Ahn;Kebede Gebeyehu Mekete;Byungjoo Kim
    • Mass Spectrometry Letters
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    • v.14 no.4
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    • pp.178-185
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    • 2023
  • QuEChERS is used worldwide as a universal sample preparation method with many benefits, such as being quick, easy, cheap, effective, rugged and safe. This study examined whether QuEChERS can be employed in isotope dilution mass spectrometry (ID-MS) for accurate analysis of pesticides in food. The ratios of fortified values and measured values of malathion and fenitrothion using the QuEChERS method were compared with those using the solid phase extract (SPE) method which was previously used in this laboratory. The separations of the two pesticides on DB-5MS and VF-1701MS columns were compared. Malathion and fenitrothion were fortified into kimchi cabbage and pretreated with the QuEChERS method and the SPE method. The results obtained using the DB-5MS column varied according to the sample preparation method, column and pesticide level. Using the VF-1701 column, ratios were 98-102% by both QuEChERS and Carb/NH2 SPE method for all fortification level. Malathion and fenitrothion were fortified into strawberry samples for comparison with kimchi cabbage. The results for the strawberry samples indicated that the ratios were not influenced by the sample preparation methods or GC column. The QuEChERS method could be acceptable in the ID-MS method for pesticide residue analysis in food, however other conditions should be carefully considered for accurate determination, such as the column, amount of analyte and food matrix.

Development of analytical method for the isotope purity of pure D2 gas using high-precision magnetic sector mass spectrometer

  • Chang, Jinwoo;Lee, Jin Bok;Kim, Jin Seog;Lee, Jin-Hong;Hong, Kiryong
    • Analytical Science and Technology
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    • v.35 no.5
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    • pp.205-211
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    • 2022
  • Deuterium (D) is an isotope with one more neutron number than hydrogen (H). Heavy elements rarely change their chemical properties with little effect even if the number of neutrons increases, but low-mass elements change their vibration energy, diffusion rate, and reaction rate because the effect cannot be ignored, which is called an isotope effect. Recently, in the semiconductor and display industries, there is a trend to replace hydrogen gas (H2) with deuterium gas (D2) in order to improve process stability and product quality by using the isotope effect. In addition, as the demand for D2 in industries increases, domestic gas producers are making efforts to produce and supply D2 on their own. In the case of high purity D2, most of them are produced by electrolysis of heavy water (D2O), and among D2, hydrogen deuteride (HD) molecules are present as isotope impurities. Therefore, in order to maximize the isotope effect of hydrogen in the electronic industry, HD, which is an isotope impurity of D2 used in the process, should be small amount. To this end, purity analysis of D2 for industrial processing is essential. In this study, HD quantitative analysis of D2 for high purity D2 purity analysis was established and hydrogen isotope RM (Reference material) was developed. Since hydrogen isotopes are difficult to analyze with general gas analysis instrument, they were analyzed using a high-precision mass spectrometer (Gas/MS, Finnigan MAT271). High purity HD gas was injected into Gas/MS, sensitivity was determined by a signal according to pressure, and HD concentrations in two bottles of D2 were quantified using the corresponding sensitivity. The amount fraction of HD in each D2 was (4518 ± 275) μmol/mol, (2282 ± 144) μmol/mol. D2, which quantifies HD amount using the developed quantitative analysis method, will be manufactured with hydrogen isotope RM and distributed for quality management and maintenance of electronic industries and gas producers in the future.

Development of analysis method for high purity nitrogen using GC-FID/Methanizer (GC-FID/Methanizer를 이용한 고순도 질소의 순도분석법 개발)

  • Jei, You;Jin Bok, Lee;Jin Seog, Kim;Woonjung, Kim;Kiryong, Hong
    • Analytical Science and Technology
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    • v.35 no.6
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    • pp.249-255
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    • 2022
  • In this study, a new method for the analysis of high-purity nitrogen was developed. A gas chromatography-flame ionization detector (GC-FID) was used for purity analysis. Certified reference materials (CRMs) at a level of 3 µmol/mol of carbon monoxide (CO), carbon dioxide (CO2), and methane (CH4), which may exist in high-purity nitrogen, were prepared using the gravimetric method, and these CRMs were used for purity analysis. In this new method, ultra-high-purity and high-purity nitrogen were used as carrier gases. The impurities in high-purity nitrogen were quantitatively analyzed by comparing the differences in the area values of the GC chromatograms of the prepared CRMs. We purchased liquid nitrogen and three bottles of nitrogen gas, which were produced by three different manufacturers, using high-purity nitrogen. Furthermore, to validate the developed purity analysis method, the fraction of impurities in high-purity nitrogen was compared with the results of the typical purity analysis method. The comparison results were consistent within the expanded uncertainties (k = 2).

Technological Trends for Precision Optical Metrology (광계측의 기술동향)

  • 김승우
    • Journal of the Korean Society for Precision Engineering
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    • v.17 no.6
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    • pp.7-16
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    • 2000
  • 정밀공학에서 측정은 필수적인 의미를 갖는다. 측정할 수 없는 제품 치수는 체계적인 가공이 불가능하며, 이는 설사 가공자의 특수한 기능에 의해 가공이 되더라도 체계적인 양산방식에 의한 생산이 될 수 없음을 의미한다. 이러한 중요성을 갖는 측정기술은 가공기술의 발랄과 더불어 꾸준한 진보를 이루어 왔다.(중략)

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