• Title/Summary/Keyword: certified reference material

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

  • Jung, Jung-Sul;Park, Jung-Woo;Yoo, Seok;Kweon, Seong-Il;Hong, Sung-Taeg;Sun, Yle-Shik;Park, Cheon-Min;Choi, Chang-Hyoo
    • Analytical Science and Technology
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    • v.25 no.5
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    • pp.273-283
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    • 2012
  • Phthalate plasticizers are regulated by RoHS, REACH and CPSC as hazardous substances. Responding to these international environmental restrictions, we developed ABS certified reference material (CRM) for determination of phthalate plasticizers such as DMP, DEP, DBP, BBP, DEHP and DnOP. The candidate material has been made with ABS resin widely used in electric and electronic products and 6 kinds of phthalate plasticizers. The making of the material involved a series of processes like extruding, cooling, pelletizing, and drying using twin screw extruder. Then it has been certified according to ISO Guide 35. Using isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS), homogeneity, short-term stability, and long-term stability were evaluated. The certified values were determined by using primary reference material (PRM) of KRISS for traceability. From now on, we will provide ABS CRM to national and international companies and research institutes after certification as certified reference material and registering on COMAR (code of reference material).

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

  • Maeng, Sae-Rom;Jin, Jong-Han;Buajarern, Jariya;Kim, Jae-Wan;Kim, Jong-Ahn;Kang, Chu-Shik
    • Journal of the Korean Society for Precision Engineering
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    • v.28 no.3
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    • pp.323-329
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    • 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
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    • v.5 no.2
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    • pp.57-61
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    • 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.

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.

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

  • 김경중;김현경;문대원;홍태은;정칠성;김이경;김재남;임철호;김정호
    • Journal of the Korean Vacuum Society
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    • v.11 no.4
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    • pp.218-224
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    • 2002
  • A domestic round robin test(RRT) for the quantitative analysis of minor impurities was performed by a standard procedure and standard reference material. The certified reference material(CRM)s for B-doped Si thin film and analysis specimens and the analysis specimens were prepared by an ion beam sputter deposition method. These samples were certified by inductively coupled plasma mass spectrometry(ICP-MS) with isotope dilution method which il one of the most quantitative methods in chemical analysis. By using an international standard procedure(ISO/DIS-l4237) for the quantitative analysis of B in Si by SIMS, a domestic RRT was performed for these specimens. Although only a few laboratories participated in this RRT, the average B concentration well agreed with the certified value within 2% error.

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 (초임계유체추출과 GC/MS를 이용한 도심 대기분진 중 PAH들의 신속한 분석법에 관한 연구)

  • Heo, Gwi Seok;Kim, Dal Ho
    • Journal of the Korean Chemical Society
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    • v.38 no.10
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    • pp.726-733
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    • 1994
  • Supercritical fluid extraction (SFE) followed by gas chromatographic separation and mass spectrometric (MS) detection were used in rapid analysis of polycyclic aromatic hydrocarbons (PAH's) in air particulate material extracted for 30 min with 10 ml of supercritical $N_2O$ without another sample preparation step. Two samples, urban dust in Seoul area and a certified air particulate reference material 1649 supplied by the NBS (National Bureau of Standards), were processed for the purpose of evaluating extraction and analysis methods. As a result, the quantitative recovery of PAH's in the SFE method was relatively lower than conventional organic solvent extraction methods, but reproducibility was resonable, and analysis time was reduced remarkably. The method has proved to be suitable for monitoring of PAH's in air particulate material.

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

  • Yu, Byung Kyu;Sun, Yle Shik
    • Journal of Environmental Analysis, Health and Toxicology
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    • v.21 no.4
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    • pp.209-219
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    • 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
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    • v.54 no.5
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    • pp.1754-1759
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    • 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.