• 제목/요약/키워드: certified reference material

검색결과 118건 처리시간 0.023초

표면분석용 인증표준물질의 개발 II : 깊이분포도용 다층 박막 표준물질의 개발 (Development of certified reference material (CRM)s for surface analysis II : multilayer thin films for sputter depth profiling)

  • 김경중;문대원
    • 한국진공학회지
    • /
    • 제8권3B호
    • /
    • pp.283-289
    • /
    • 1999
  • Multilayer thin film reference materials for the sputter depth profiling analysis are used to calibrate the sputter depth scale by measuring the sputtering rate and to optimize the sputtering conditions for the best depth resolution. Surface analysis group of Korea Research Institute of Standards and science (KRISS) have developed various types of multilayer thin films by using an ion beam sputter deposition and in-situ surface analysis system. The chemical states of the thin films reference materials were certified by in-situ XPS and the thicknesses were certified by transmission electron microscopy (TEM).

  • PDF

ABS 중 phthalates 가소제 CRM 개발에 대한 연구 (A study on the development of phthalate plasticizers CRM in ABS resin)

  • 정정설;박정우;유석;권성일;홍성택;선일식;박천민;최창휴
    • 분석과학
    • /
    • 제25권5호
    • /
    • pp.273-283
    • /
    • 2012
  • 현재 RoHS 및 REACH, CPSC 등에서 phthalates 가소제를 유해물질로 분류하여 규제하고 있는 실정이다. 이러한 국제환경규제에 대응하기 위해 phthalates 가소제 정량분석용 ABS 인증표준물질을 개발하였으며 인증 대상물질은 DMP, DEP, DBP, BBP, DEHP, DnOP이다. 후보물질은 전기 전자제품에 많이 사용되고 있는 ABS 수지에 phthalates 가소제 6가지 물질을 혼합한 후 쌍축압출기(twin screw extruder)를 이용하여 압출, 냉각, 펠렛, 건조의 과정을 거쳐 제조하였으며 ISO Guide 35의 절차에 따라 인증하였다. 동위원소희석 질량분석법(ID-GC/MS)을 이용하여 균질성, 단기안정성 및 장기안정성을 평가하였으며, 소급성 확립을 위해 한국표준과학연구원(KRISS)의 일차표준물질을 이용하여 인증값을 결정하였다. 향후 인증표준물질로서 인증을 받은 후, 국제 표준물질 데이터베이스(COM AR:code of reference material)에 등록하고 국내 외 산업체 및 시험기관에 보급할 예정이다.

다중 프로브 검사 계측 장비를 위한 단차 표준 인증 물질의 설계 및 제작 (Design and Fabrication of a Step Height Certified Reference Material for Multi-probe Inspection Instruments)

  • 맹새롬;진종한;;김재완;김종안;강주식
    • 한국정밀공학회지
    • /
    • 제28권3호
    • /
    • pp.323-329
    • /
    • 2011
  • Certified reference materials (CRMs) have been used to calibrate surface profilers for reliable measurements. In this paper, we present a newly designed step height CRM which has a step height pattern with two different widths and various special patterns for checking radial magnification, distortion of optical viewing systems, etc. Especially, it could be useful for multi-probe inspection instruments in the manufacturing lines. The fabrication was done by conventional optical lithography and dry etching process with optimized conditions. To verify the step height values, a white-light scanning interferometer was used with objective lenses having magnification of $10{\times}$ and $100{\times}$. CRMs with nominal step heights of $0.5\;{\mu}m$, $1\;{\mu}m$, $3\;{\mu}m$, $5\;{\mu}m$, $7\;{\mu}m$, and $10\;{\mu}m$ were fabricated and the uniformity of these CRMs was evaluated to be less than 3 nm ($1{\sigma}$).

Accurate Measurement of Arsenic in Laver by Gravimetric Standard Addition Method Combined with High Resolution Inductively Coupled Plasma Mass Spectrometry

  • Lee, Kyoung-Seok;Kim, Hyeon-Ji;Yim, Yong-Hyeon;Kim, Jeongkwon;Hwang, Euijin
    • Mass Spectrometry Letters
    • /
    • 제5권2호
    • /
    • pp.57-61
    • /
    • 2014
  • A gravimetric standard addition method combined with internal standard calibration has been successfully developed for the accurate analysis of total arsenic in a laver candidate reference material. A model equation for the gravimetric standard addition approach using an internal standard was derived to determine arsenic content in samples. Handlings of samples, As standard and internal standard were carried out gravimetrically to avoid larger uncertainty and variability involved in the volumetric preparation. Germanium was selected as the internal standard because of its close mass to the arsenic to minimize mass-dependent bias in mass spectrometer. The ion signal ratios of $^{75}As^+$ to $^{72}Ge^+$ (or $^{73}Ge^+$) were measured in high resolution mode ($R{\geq}10,000$) to separate potential isobaric interferences by high resolution ICP/MS. For method validation, the developed method was applied to the analysis of arsenic content in the NMIJ 7402-a codfish certified reference material (CRM) and the result was $37.07mg{\cdot}kg^{-1}{\pm}0.45mg{\cdot}kg^{-1}$ which is in good agreement with the certified value, $36.7mg{\cdot}kg^{-1}{\pm}1.8mg{\cdot}kg^{-1}$. Finally, the certified value of the total arsenic in the candidate laver CRM was determined to be $47.15mg{\cdot}kg^{-1}{\pm}1.32mg{\cdot}kg^{-1}$ (k = 2.8 for 95% confidence level) which is an excellent result for arsenic measurement with only 2.8 % of relative expanded uncertainty.

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

  • 김영희;송기봉;신선경;이정섭;정기택;홍은진;박진주;유석민
    • 분석과학
    • /
    • 제23권3호
    • /
    • pp.295-303
    • /
    • 2010
  • 폐수 시료를 이용한 중금속분석용 수질표준물질을 제조하여, 납, 카드뮴, 크롬, 구리, 아연, 망간, 철 등 중금속 7 종에 대해 인증분석 및 불확도 등을 평가하고, 24 개 환경측정분석기관을 대상으로 실험실간 비교실험을 실시하였다. 폐수표준물질의 인증값 및 확장불확도는 KS A ISO 가이드 35(2005)에 의해 도출하였으며, 균질성에 기인한 표준불확도는 특성값의 0.43~2.67%로 나타났다. 환경측정분석기관간 비교실험에서 모든 항목의 비교실험 결과값이 정규분포를 따랐으며, 로버스트 평균값과 폐수표준물질의 인증값과 비교한 결과, 대부분의 항목에서 로버스트 평균값이 인증값보다 낮게 나타났다.

실리콘에 도핑된 붕소의 정량분석에 대한 공동분석연구 (RRT Study for the Quantitative Analysis of Boron in Silicon)

  • 김경중;김현경;문대원;홍태은;정칠성;김이경;김재남;임철호;김정호
    • 한국진공학회지
    • /
    • 제11권4호
    • /
    • pp.218-224
    • /
    • 2002
  • 반도체 박막의 분석에서 중요한 분석 대상의 하나인 미량 불순물의 정량분석을 위한 표준절차를 확립하고 그에 필요한 인증표준물질의 개발하였으며 이를 이용하여 국내공동분석을 실시하였다. 공동분석에 사용된 붕소가 균질하게 도핑된 박막 인증표준물질과 분석시편은 이온빔 스퍼터증착법에 의해 제작하였으며, 가장 정량적이고 감도가 높은 ICP-MS를 이용한 동위원소희석법으로 인증하였다. 이러한 인증표준물질과 SIMS에 의한 실리콘 내 의 붕소의 정량분석에 대해 이미 확립되어 있는 국제표준절차인 ISO/DIS-14237에 의거하여 국내 공동 분석을 시행하였는데, 이번의 공동분석에서 얻어진 붕소농도의 전체 평균값이 ICP-MS에 의한 인증치에 약 2% 정도의 오차를 보여주고 있어 분석의 정확성이 확인되었다.

초임계유체추출과 GC/MS를 이용한 도심 대기분진 중 PAH들의 신속한 분석법에 관한 연구 (A Rapid Method for Analysing Polycyclic Aromatic Hydrocarbons (PAH's) in Urban Dust Using Supercritical Fluid Extraction (SFE) and Gas Chromatography/Mass Spectrometry (GC/MS)허귀석, 김달호)

  • 허귀석;김달호
    • 대한화학회지
    • /
    • 제38권10호
    • /
    • pp.726-733
    • /
    • 1994
  • 대기부유분진(air particulate material)중에 존재하는 다환방향족탄화수소(polycyclic aromatic hydrocarbons, PAH)를 신속하고 정확하게 분석하기 위하여 대기부유분진 시료를 10ml의 초임계유체($N_2O$ )로 30분간 추출 후 별도의 전처리와 농축과정 없이 GC/MS에서 분석하여 분석시간과 분석과정을 단축 및 단순화하였다. 시료로서 NBS 대기부유분진 인증표준기준물질(certified particulate reference material, CRM)1649와 서울의 도심에서 채취한 대기부유분진 시료를 이용하여 기존의 추출법 및 분석방법과 비교하였다. 그 결과 본 분석방법은 기존의 분석법에 비해 회수율은 상대적으로 작았으나 재현성이 좋았으며 분석과정이 간단하고 분석시간이 현저히 단축됨을 알 수 있었다.

  • PDF

환경규제 대응을 위한 페인트 중의 중금속 분석용 인증 표준물질 개발 (Development of Certified Reference Materials for Analysis of Heavy Metals in Paints to Cope with Environmental Regulations)

  • 유병규;선일식
    • 환경분석과 독성보건
    • /
    • 제21권4호
    • /
    • pp.209-219
    • /
    • 2018
  • In the areas of RoHS, WEEE, ELV and REACH, reinforcement of environmental regulations against harmful substances is a global trend not only in EC but also in all over the world. In the fields of Korea's major export products such as material parts, electrical and electronic products and automobile parts, we are responding to these regulations consistently. To develop reference material for analyzing lead and cadmium in paints, the candidate materials were produced through the screening process which separated shapes and sizes. To secure the traceability of the candidate materials produced, the characteristics and uncertainties are estimated by ICP-AES analysis using the primary reference material. The short-term and long-term stabilities also are evaluated in parallel. In order to calculate the final certification value of the candidate material, the verification were carried out by the performance evaluation through the comparison among the KOLAS (Korea Laboratory Accreditation Scheme) laboratories, and the CRM was produced in accordance with ISO Guide 35. The certified values and uncertainties of Pb and Cd of the final paint standard, determined according to the joint analysis among laboratories, are Pb [($191.4{\pm}3.1$) mg/kg, ($944.1{\pm}5.6$) mg/kg] and Cd [($45.0{\pm}2.6$) mg/kg, ($225.5{\pm}3.5$) mg/kg]. These standard materials were developed to enhance the reliability of measurement analysis, including the validity and traceability of measurement results. Also it is expected that the CRM will be used as QCM (quality control material) for the product design and the process monitoring, so that regulation and management of hazardous heavy metals can be systematically implemented.

Source and LVis based coincidence summing correction in HPGe gamma-ray spectrometry

  • Lee, Jieun;Kim, HyoJin;Kye, Yong Uk;Lee, Dong Yeon;Kim, Jeung Kee;Jo, Wol Soon;Kang, Yeong-Rok
    • Nuclear Engineering and Technology
    • /
    • 제54권5호
    • /
    • pp.1754-1759
    • /
    • 2022
  • The activity of gamma-ray emitting nuclides is calculated assuming that each gamma-ray is detected individually; thus, the magnitude of the coincidence summing signal must be considered during activity calculations. Here, the correction factor for the coincidence summing effect was calculated, and the detection efficiencies of two HPGe detectors were compared. The CANBERRA Inc. GC4018 high-purity Ge detector provided an estimate for the peak-to-total ratio using a point source to determine the coincidence summing correction factor. The ORTEC Inc. GEM60 high-purity Ge detector uses EFFTRAN in LVis to obtain the parameters of the detector and source model and the gamma-gamma and gamma-X match estimates, in order to determine the coincidence summing correction factor. Nuclide analyses, radioactivity comparisons, and analyses of reference material samples were performed utilizing certified reference materials to accurately determine the detection efficiencies. For both Co-60 and Y-88, the detection efficiency for a point source increased by an average of at least 12-13%, whereas the detection efficiency determined using LVis increased by an average of at least 13-15%. The calculated radioactivity values of the certified reference material and reference material samples were accurate to within 3% and 6% of the measured values, respectively.