• 제목/요약/키워드: internal standard method

검색결과 696건 처리시간 0.029초

후 컬럼 동위원소 희석법을 적용한 HPLC-ICP/MS에서의 정량분석에서 내부 표준물을 이용한 정확도와 정밀도의 개선연구 (Study of improving precision and accuracy by using an internal standard in post column isotope dilution method for HPLC-ICP/MS)

  • 주민규;박명순;박용남
    • 분석과학
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    • 제27권3호
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    • pp.140-146
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    • 2014
  • 후 컬럼 동위원소 희석법(PCID, post column isotope dilution)을 HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry)에 적용한 정량법에서 내부 표준물을 동시에 사용하여 정확도와 정밀도를 개선하였다. 전통적인 여러 정량법과 후 컬럼 동위원소 희석법을 비교하여 볼 때에 PCID의 경우에 컬럼내에서 발생하는 오차가 가장 큰 요인으로 작용하였음을 알 수 있었다. PCID에서 내부 표준물을 사용하여 컬럼내에서의 손실에 대한 오차를 효과적으로 보정하고 정확도와 정밀도를 개선할 수 있었다. 셀레늄 화학종인 SeMet을 시료로 사용하고 내부 표준물로 MeSecys 또는 $Se^{4+}$를 이용한 결과, 사용하지 않은 경우와 비교하면 상대오차는 각 각 31%와 13%에서 모두 1% 대로 낮아져 정확도가 크게 개선되었으며, 상대 표준편차는 5.1%와 6.9%에서 각각 1.5%와 0.2%로 정밀도 또한 크게 개선되었다. PCID에서 내부 표준물을 사용하였을 때의 정량분석법의 장점을 다른 분석법과 비교 토의하였다.

외부표준법을 적용한 토양시료의TXRF 정량분석 정확도 개선 (Improvement of accuracy in quantitative TXRF analysis of soil sample by applying external standard method)

  • 박진규;박난희;한선호;임상호;이치규;송규석
    • 분석과학
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    • 제29권6호
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    • pp.261-268
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    • 2016
  • TXRF는 시료전처리 없이 분말상 시료의 정량분석이 가능하여 토양시료를 효율적으로 분석할 수 있다. 기존의 내부표준법을 이용한 분석법은 매질 효과 및 형광신호의 겹침으로 인한 간섭 효과로 인해 정확도가 떨어진다. 이를 개선하기 위해 외부표준법을 적용하여 용액화한 토양시료와 분말상 토양시료를 분석하였다. 용액화한 토양시료의 경우 개별표준물질로 만든 표준용액으로 작성한 검량선으로 분석하였는데, 내부 및 외부표준법 간 유의미한 차이가 없었다. 반면 분말상 토양시료로 부유용액을 만들어 검량선을 작성한 후 이를 이용하여 분말상 토양시료를 분석한 결과, 전반적으로 외부표준법을 적용한 결과가 내부표준법의 그것에 비해 정확도가 높았다. 두 가지 표준토양시료로 교차검증한 결과, Al, Fe, K, Ca, Ti, Ba, Mn, Sr, Rb, Cu 등 10개의 원소들에 대해 ${\pm}20%$ 내외의 상대오차가 측정되었다.

갑상선 기능 항진증 변증 도구 개발 기초 연구 (Development of a Basic Standard Tool for Pattern Identification in Hyperthyroidism)

  • 최유진;한양희;안세영;조충식;신선미
    • 대한한방내과학회지
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    • 제39권6호
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    • pp.1256-1271
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    • 2018
  • Objective: The purpose of this study was to develop a basic standard tool for pattern identification in hyperthyroidism. Method: It was based on a review of the published literature in China and Korea. The advisory committee on this study included 8 internal medicine professors from Korean Medicine Schools and 2 who had a doctor's degree and specialized in internal medicine. We were advised about the importance of pattern identification, weight gain as a symptom, the importance of treatment, changes in symptoms, rare changes in symptoms, and frequency of prescriptions regarding hyperthyroidism. Results: A Korean instrument of pattern identification was completed. Conclusion: We sincerely look forward to improving the instrument through continuous clinical studies.

소규모 하천 친환경 물흐름을 위한 차수특성 (Waterproof Characteristic for Environmental Water Flows in Small Streams)

  • 박민철;김성구;이송
    • 한국지반공학회:학술대회논문집
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    • 한국지반공학회 2010년도 추계 학술발표회 2차
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    • pp.192-199
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    • 2010
  • This research produced internal model tester ($2.0m{\times}2.0m{\times}1.0m$) to evaluate the field application of Paju Unjeong District water recycling system for small streams eco-friendly river bed disparity method for the first time in Korea and conducted comparative analysis of the Paju Unjeong District water recycling system field test results and infiltration rate result of internal tests by each rainfall intensity following surface material. Infiltration rate result of internal tests concrete pavement by rainfall intensity following surface material, asphalt pavement, bentonite mate, stabilized soil construction and mixed soil construction manifested low infiltration rate. On the contrary, compaction soil, grassland and water permeable packaging materials resulted in significant amount of infiltration rate. As for the field permeability test results, they were manifested similar tendency as indoor permeability test results and they satisfied the standard for standard of water permeability of domestic disparity facility (less than $1.0{\times}10-7cm$/sec). As compaction rate increased, unconfined compression strength increased as well while coefficient of water permeability decreased.

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Comparison of results between modified-Angoff and bookmark methods for estimating cut score of the Korean medical licensing examination

  • Yim, Mikyoung
    • Korean journal of medical education
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    • 제30권4호
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    • pp.347-357
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    • 2018
  • Purpose: The purpose of this study was to apply alternative standard setting methods for the Korean Medical Licensing Examination (KMLE), a criterion-referenced written examination, and to compare them to the conventional cut score used on the KMLE. Methods: The process and results of criterion-referenced standard settings (i.e., the modified-Angoff and bookmark methods) were evaluated. The ratio of passing and failing examinees determined using these alternative standard setting methods was compared to the results of the conventional criteria. Additionally, the external, internal and procedural evaluation of these methods were reviewed. Results: The modified-Angoff method yielded the highest cut score, followed sequentially by the conventional method and the bookmark method. The classification agreement between the modified-Angoff and bookmark methods was 0.720 measured by Cohen's ${\kappa}$ coefficient. The intra-panelist classification consistency of modified-Angoff method was higher than bookmark method. However, the inter-panelist classification consistency was vice versa. The standard setting panelists' survey results showed that the procedures of both methods were satisfactory, but panelists had more confidence in the results of the modified-Angoff method. Conclusion: The modified-Angoff method showed results that were more similar to those of the conventional method. Both new methods showed very high concordance with the conventional method, as well as with each other. The modified-Angoff method was considered feasible for adoption on the KMLE. The standard setting panelists responded positively to the modified-Angoff method in terms of its practical applicability, despite certain advantages of the bookmark method.

Free vibrations of arbitrary quadrilateral thick plates with internal columns and uniform elastic edge supports by pb-2 Ritz method

  • Wu, L.H.
    • Structural Engineering and Mechanics
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    • 제44권3호
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    • pp.267-288
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    • 2012
  • Free vibration analysis of arbitrary quadrilateral thick plates with internal columns and elastic edge supports is presented by using the powerful pb-2 Ritz method and Reddy's third order shear deformation plate theory. The computing domain of arbitrary quadrilateral planform is mapped onto a standard square form by coordinate transformation. The versatile pb-2 Ritz functions defined by the product of a two-dimensional polynomial and a basic function are taken to be the admissible functions. Substituting these displacement functions into the energy functional and minimizing the total energy by differentiation, leads to a typical eigenvalue problem, which is solved by a standard eigenvalue solver. Stiffness and mass matrices are numerically integrated over the plate by using Gaussian quadrature. The accuracy and efficiency of the proposed method are demonstrated through several numerical examples by comparison and convergency studies. A lot of numerical results for reasonable natural frequency parameters of quadrilateral plates with different combinations of elastic boundary conditions and column supports at any locations are presented, which can be used as a benchmark for future studies in this area.

Buckling of aboveground oil storage tanks under internal pressure

  • Yoshida, Shoichi
    • Steel and Composite Structures
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    • 제1권1호
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    • pp.131-144
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    • 2001
  • Overpressurization can occur due to the ignition of flammable vapors existing inside aboveground oil storage tanks. Such accidents could happen more frequently than other types of accident. In the tank design, when the internal pressure increases, the sidewall-to-roof joint is expected to fail before failure occurs in the sidewall-to-bottom joint. This design concept is the socalled "frangible roof joint" introduced in API Standard 650. The major failure mode is bifurcation buckling in this case. This paper presents the bifurcation buckling pressures in both joints under internal pressure. Elastic and elastic-plastic axisymmetric shell finite element analysis was performed involving large deformation in the prebuckling state. Results show that API Standard 650 does not evaluate the frangible roof joint design conservatively in small diameter tanks.

HPLC-UV를 이용한 땃두릅나무 줄기의 지표 성분 동시 분석법 확립 (Establishment of HPLC-UV Analysis Method Validation for Simultaneous Analysis of Standard Compounds of Oplopanax elatus Nakai Stem)

  • 유남호;권용수;김명조
    • 생약학회지
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    • 제50권2호
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    • pp.133-140
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    • 2019
  • In our previous study, we found uracil, adenosine, protocatechuic acid, syringin (eleutheroside B) and scoparone (6, 7-dimethoxycoumarin) in the Oplopanax elatus Nakai Stem. High-performance liquid chromatography (HPLC) -UV was used to quality and quantify the internal marker compounds in the O. elatus extract after validation of method with linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy and precision. The specificity assessment visually confirmed that the substance was detected without the introduction of other substances. The established method showed high linearity of the calibration curve and coefficient of correlation ($R^2$) of over the 0.999. HPLC was reported as five standard compounds equivalent using the following linear equation based on the calibration curve. The accuracy of measurement was 84.34 ~ 119.74% and the relative standard deviation (RSD) value was 0.28 ~ 1.60%. In addition, our established method showed high repeatability. The RSD value was 1.10 ~ 6.81%. So, we found the amount of the internal marker compounds in the O. elatus extract. These results demonstrated that can be used to quality evaluation of the O. elatus.

Use of Nuclear Magnetic Resonance Spectroscopy in Analysis of Fennel Essential Oil

  • AbouZid, Sameh
    • Natural Product Sciences
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    • 제22권1호
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    • pp.30-34
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    • 2016
  • A simple and rapid method based on proton nuclear magnetic resonance spectroscopy was developed for determination of trans-anethole content in fennel essential oil. Spectra of pure trans-anethole, of the pure essential oil of fennel, and of the pure oil of fennel with thymol internal standard were recorded. The signal of $H-1^/$ was used for quantification of trans-anethole. This proton signal is well separated in the proton magnetic resonance spectrum of the compound. No reference compound is needed and cheap internal standard was used. The results obtained from spectroscopic analysis were compared with those obtained by gas chromatography. Additionally, the developed method was used for determination of the type of vegetable oil used as a carrier in commercial products, which cannot be quantified as such by gas chromatography. This study demonstrates the application of proton nuclear magnetic resonance spectroscopy as a quality control method for estimation of essential oil components.

ESR 자동분석기를 이용한 내부정도관리방법 (The Internal Quality Control for TEST 1, the Automatic Analyzer of Erythrocyte Sedimentation Rate)

  • 조영국;심현설;송운흥;박규은
    • 대한임상검사과학회지
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    • 제36권2호
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    • pp.239-244
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    • 2004
  • Recently automatic equipment has been well popularized for the erythrocyte sedimentation rate, a widely used test, but no standard quality control has been established yet. Thus, we are going to report a case that established and applied a quality control method using the TEST 1 automatic analyzer. For internal quality control, we adopted the repeatability test through comparison with daily mean check, with a manual method using patients' specimens and with the results of a test on the previous day. In order to set the tolerance standard for each quality control method, we compared the results of 50 specimens that showed a wide range of ESR results and examined correlation and differences according to result. After setting the tolerance standard, we applied the standard at tertiary university hospitals for 120 days and investigated positive rates and re-examination rates. If the tolerance standard was exceeded, the cause was also identified. We selected a specimen of below 25 mm/hr (T1), one between 26-50 mm/hr (T2) and one of over 51 mm/hr (T3) at random. The correlation between the manual method and the automatic method was quite high (r=0.98), and it is found appropriate to set based on differences in result values below 25 mm/hr, the upper limit of the reference value, and based on differences in the percentage of result values above 25 mm/hr. Accordingly, we set the criteria for rejection above 10 mm/hr and above 20%. When the criteria were applied in the laboratory, 1.7% of specimens in the range of T1, 8.3% of those in the range of T2 and 7.5% of those in the range of T3 were rejected. Because all the rejected ones fell within the tolerance limit in re-examination calibration verification was not carried out. With the wide popularization of erythrocyte sedimentation rate analyzers that can carry out a lot of tests quickly using automatic methods, it is necessary to improve the reliability of test results by establishing internal quality control policies. We expect that an agreed standard quality control method may be established based on the method proposed in this study.

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