• Title/Summary/Keyword: reference materials

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미량원소분석을 위한 쌀분말 기준물질의 제조 및 검정 (Preparation and Certification of Rice Flour Reference Materials for Trace Elements Analysis)

  • 조경행;박창준;우진춘;서정기;한명섭;이종해
    • 분석과학
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    • 제11권4호
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    • pp.271-280
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    • 1998
  • 국내에서 재배 생산된 현미로 부터 표준물질을 가공하여 원소별 검정분석을 실시하였다. 주요 오염원소의 농도가 서로 다른 2종의 쌀분말 표준물질을 제조하였는데 1종은 정상치시료로서 분말 시료를 그대로 처리하였으며, 1종은 제조과정중에 As, Cu, Pb, Hg, Cr, Cd등 6개의 중금속원소를 건조중량기준 $1.0{\mu}g/g$씩 첨가한 고농도 오염시료로서 제조하였다. 제조된 시료는 중성자방사화분석법 (NAA)과 불꽃원자흡수분광법(FAAS)으로 Cd, Cu, Fe, Mn, Zn등 5개 원소에 대한 균질도 분석을 실시하여 기준불질로서의 균질성을 확인하였다. 쌀시료의 분해 및 전처리에는 고온가압법과 마이크로파분 해법을 사용하였으며, NAA, FAAS, 흑연로원자흡수분광법(GFAAS), 유도플라즈마방출분광법(ICP-AES), 동위원소희석질량분석법(IDMS), 증기발생법 등을 이용하여 쌀분말표준물질 소재의 원소별 정량 분석을 실시하였다. 이들 각 방법의 원소별 분석결과를 이용하여 P, K, Mg, As, Ca, Cd, Cr, Cu, Fe, Mn, Mo, Na, Zn, Pb, Se, Hg등 16개 원소에 대한 검정값 및 참고값을 확정하였다.

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동위원소희석 유도결합플라스마질량분석법에 의한 저 합금강 표준시료중의 Ni, Cr, Mo의 분석 (Determination of Ni, Cr, Mo in Low Alloy Steel Reference Materials by Isotope Dilution Inductively Coupled Plasma Mass Spectrometry)

  • 서정기;우진춘;민형식;임명철
    • 분석과학
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    • 제16권1호
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    • pp.82-89
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    • 2003
  • Isotope dilution mass spectrometry (IDMS) was applied to the determination of Ni, Cr, Mo in low alloy steel reference materials. The Mo isotope ratio measurement was performed by dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP/MS) using ammonia as a reaction cell gas. In the case of Ni and Cr measurement, all data were obtained at medium resolution mode (m/${\Delta}m=3000$) of double focusing sector field high resolution inductively coupled plasma mass spectrometry (HR-ICP/MS). For the method validation of the technique was assessed using the certified reference materials such as NIST SRM 361, NIST SRM 362, NIST SRM 363, NIST SRM 364, NIST SRM 36b. This method was applied to the determination of Ni, Cr and Mo in low alloy steel sample (CCQM-P25) provided by NMIJ for international comparison study.

초정밀 유정압 테이블에서 냉각장치의 변수 설정이 온도특성에 미치는 영향 (Influence of Parameter Setting in an Oil Cooler on the Temperature Characteristics of an Ultra-precision Hydrostatic Table)

  • 김경호;김창주;오정석;박천홍
    • 한국정밀공학회지
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    • 제32권6호
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    • pp.571-576
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    • 2015
  • Temperature characteristics of supply oil in an ultra-precision hydrostatic table are largely influenced by parameter setting in an oil cooler such as the location of reference sensor and cooling temperature. In this paper, influences of the parameter setting on the temperature variation in the hydrostatic table are experimentally analyzed to suggest the guidelines for practical application. In case of using temperature of inlet oil as a reference sensor in the oil cooler, temperature rise of the supply oil is smaller and thermal settling time is faster than that of using temperature of outlet oil as a reference sensor. The experimental results also show that temperatures of table, rail and return oil can be made almost same, and thermal settling time can be decreased by setting cooling temperature in the oil cooler to be lower than atmospheric temperature.

Validation of Radioanalytical Techniques for Nuclear Waste Characterisation

  • Warwick, Phillip E.
    • 방사성폐기물학회지
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    • 제17권4호
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    • pp.363-373
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    • 2019
  • Waste characterisation associated with nuclear site decommissioning relies on radiochemical analysis of a diverse range of sample types, requiring extensive validation of analytical techniques using matrix-matched materials. The absence of relevant reference materials has hindered robust method development and validation. The paper discusses how method validation in support of nuclear waste characterisation can be achieved without using reference materials. The key stages in an analytical procedure are evaluated and a multi-stage approach is proposed with the ultimate aim of determining an operational envelope for an analytical procedure.

Reference Electrode for Monitoring Cathodic Protection Potential

  • Panossian, Z.;Abud, S.E.
    • Corrosion Science and Technology
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    • 제16권5호
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    • pp.227-234
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    • 2017
  • Reference electrodes are generally implemented for the purpose of monitoring the cathodic protection potentials of buried or immersed metallic structures. In the market, many types of reference electrodes are available for this purpose, such as saturated calomel, silver/silver chloride and copper/copper sulfate. These electrodes contain a porous ceramic junction plate situated in the cylindrical body bottom to permit ionic flux between the internal electrolyte (of the reference electrode) and the external electrolyte. In this work, the copper/copper sulfate reference electrode was modified by replacing the porous ceramic junction plate for a metallic platinum wire. The main purpose of this modification was to avoid the ion copper transport from coming from the inner reference electrode solution into the surrounding electrolyte, and to mitigate the copper plating on the coupon surfaces. Lab tests were performed in order to compare the performance of the two mentioned reference electrodes. We verified that the experimental errors associated with the measurements conducted with developed reference electrode would be negligible, as the platinum surface area exposed to the surrounding electrolyte and/or to the reference electrolyte are maintained as small as possible.

Determination of trace elements in food reference materials by instrumental neutron activation analysis

  • Cho, K.H.;Zeisler, R.;Park, K.W.
    • 분석과학
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    • 제18권6호
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    • pp.520-528
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    • 2005
  • Two biological Certified Reference Materials (CRMs), KRISS 108-04-001 (oyster tissue) and 108-05-001 (water dropwort stem), were prepared by Korea Research Institute of Standards and Science (KRISS)during FY '01. The certified values of these materials had been determined by Isotope Dilution Mass Spectrometry (IDMS) for six elements (Cd, Cr, Cu, Fe, Pb and Zn). Additional analytical works are now progressing to certify the concentrations of a number of the environmental and nutrimental elements in these CRMs. The certified values in a CRM are usually determined by using a single primary method with confirmation by other method(s) or using two independent critically-evaluated methods. Instrumental Neutron Activation Analysis (INAA) plays an important role in the determination of certified values as it can eliminate the possibility of common error sources resulting from sample dissolution. In this study INAA procedure was used in determination of 23 elements in these two biological CRMs to acquire the concentration information and the results were compared with KRISS certified values.

배관 내 축방향 반타원 표면균열에 대한 비선형 파괴역학 해석 (Non-Linear Fracture Mechanics Analyses for Axial Semi-Elliptical Surface Cracked Pipes)

  • 김진수;김윤재;김영진
    • 대한기계학회:학술대회논문집
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    • 대한기계학회 2003년도 춘계학술대회
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    • pp.143-148
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    • 2003
  • This paper provides two types of engineering J estimation equations for cylinders with finite internal axial surface cracks under internal pressure. The first type is the so-called GE/EPRI type J estimation equation based on Ramberg-Osgood materials. Based on detailed 3-D FE results the GE/EPRI-type J estimation equation along the crack front is proposed and validated for Ramberg-Osgood materials. For more general application, the developed GE/EPRI-type solutions are then re-formulated based on the reference stress concept. The proposed reference stress based J estimation equation has good agreement between the FE results and the proposed reference stress based J estimation provides confidence in the use of the proposed method for elastic-plastic fracture mechanics of pressurised piping

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불화물을 이용한 산소센서의 제조및 특성 (Fabrication and Characteristics of Oxygen Gas Sensor using Fluoride Compaunds)

  • 이재현;홍영호;장동근;이병택;김태훈;이덕동
    • 한국재료학회:학술대회논문집
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    • 한국재료학회 1993년도 추계 학술발표 강연 및 논문 개요집
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    • pp.69-71
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    • 1993
  • Fluoride compound potentiometric cell oxygen sensors were fabricated for the measurement of oxygen pressure in the low temperature range (300。K-500。K). The disk type sensors consist of a reference Air(0$_2$):Ag, a solid electrolyte SrF$_2$, and a sensing metel Ag electrode. And the buried reference electrode type sensor have a NiO/Ni reference electrode. The open circuit emf of the cell showed high sensivity to oxygen gas (60mv) at the measuring temperature 20$0^{\circ}C$. Also, The buried reference electrode type sensor showed 30mv from 1% to 10% oxygen pressure range.

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웨이퍼 그라인딩 공정으로 생성된 스크래치 마크를 갖는 실리콘 칩들에서의 벽개 파괴현상 (Cleavage Fracture Phenomenon in Silicon Chips with Wafer Grinding-Induced Scratch Marks)

  • 이동기;이태규;이성민
    • 대한금속재료학회지
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    • 제49권9호
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    • pp.726-731
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    • 2011
  • The present work shows how the flexural displacement-induced fracture strength of silicon devices, whose back surfaces have wafer grinding-induced scratch marks, depends on the crystallographic orientation. Experimental results indicate that silicon devices with scratch marks parallel to their lateral direction (i.e. reference axis in this work) are very susceptible to flexural fracture, as compared to devices with marks which deviated from the direction. The 3-point bending test shows that the fracture strength of silicon devices having marks which are oriented away from the reference axis is 2.6 times higher than that of devices with marks parallel to the axis. It was particularly interesting to see that silicon devices with identical preferred marks even reveal different fracture strengths, depending on whether the marks are involved in specific crystal planes such as {111} or {011}, called cleavage planes. This work demonstrates that silicon devices with the reference axis-aligned scratch marks not existing on such cleavage planes can have higher fracture strength approximately 20% higher than those existing on the planes.

Characterizing a Full Spectrum of Physico-Chemical Properties of Ginsenosides Rb1 and Rg1 to Be Proposed as Standard Reference Materials

  • Kim, Il-Woung;Hong, Hee-Do;Choi, Sang-Yoon;Hwang, Da-Hye;Her, Youl;Kim, Si-Kwan
    • Journal of Ginseng Research
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    • 제35권4호
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    • pp.487-496
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    • 2011
  • Good manufacturing practice (GMP)-based quality control is an integral component of the common technical document, a formal documentation process for applying a marketing authorization holder to those countries where ginseng is classified as a medicine. In addition, authentication of the physico-chemical properties of ginsenoside reference materials, and qualitative and quantitative batch analytical data based on validated analytical procedures are prerequisites for certifying GMP. Therefore, the aim of this study was to propose an authentication process for isolated ginsenosides $Rb_1$ and $Rg_1$ as reference materials (RM) and for these compounds to be designated as RMs for ginseng preparations throughout the world. Ginsenoside $Rb_1$ and $Rg_1$ were isolated by Diaion HP-20 adsorption chromatography, silica gel flash chromatography, recrystallization, and preparative HPLC. HPLC fractions corresponding to those two ginsenosides were recrystallized in appropriate solvents for the analysis of physico-chemical properties. Documentation of the isolated ginsenosides was made according to the method proposed by Gaedcke and Steinhoff. The ginsenosides were subjected to analyses of their general characteristics, identification, purity, content quantitation, and mass balance tests. The isolated ginsenosides were proven to be a single compound when analyzed by three different HPLC systems. Also, the water content was found to be 0.940% for $Rb_1$ and 0.485% for $Rg_1$, meaning that the net mass balance for ginsenoside $Rb_1$ and $Rg_1$ were 99.060% and 99.515%, respectively. From these results, we could assess and propose a full spectrum of physicochemical properties for the ginsenosides $Rb_1$ and $Rg_1$ as standard reference materials for GMP-based quality control.