• Bulletin of the Korean Chemical Society
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• v.35 no.3
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• pp.821-827
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• 2014

An isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) method has been developed and applied to the determination of arsenobetaine (AsB, ${(CH_3)_3}^+AsCH_2COO^-$) from oyster candidate certified reference material (CRM). The exact matching isotope dilution approach was adopted for accurate determination of AsB using $^{13}C_2$-labeled AsB as an internal standard. Efficiencies of different AsB extraction methods were evaluated using a codfish reference material and a simple sonication method was selected as the method of choice for the certification of the oyster candidate CRM. The hydrophilic interaction liquid chromatography (HILIC) combined with electrospray ionization tandem mass spectrometry (ESI/MS/MS) in selected reaction monitoring (SRM) mode was optimized for adequate chromatographic retention and robust quantification of AsB from codfish and oyster samples. By analyzing 12 subsamples taken from each 12 bottles systematically selected from the whole oyster CRM batch, the certified value of AsB was determined as $6.60mg{\cdot}kg^{-1}{\pm}0.31mg{\cdot}kg^{-1}$ and it showed excellent between-bottle homogeneity of less than 0.42%, which is represented by relative standard deviation of 12 bottles from the CRM batch. The major source of uncertainty was the certified value of the AsB standard solution.

• The Korean Journal of Nuclear Medicine Technology
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• v.18 no.1
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• pp.158-162
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• 2014

Purpose: Reference material (RM) is defined as material that is safe and homogeneous enough about specified characteristic that is made with a purpose of using test of measurement or nominal characteristic. Certified reference material (CRM), which is issued by authorized organization, is defined as reference material that provides characteristic value, link uncertainty and retroactivity. The purpose of this paper was to evaluate recovery of radioimmunoassay by Certified Reference Material enclosed with a certificate and therefore to enhance reliability of test. Materials and Methods: WHO certified reference material is purchased from NIBSC (National Institute for Biological Standard and Control, United Kingdom) and made of 3 levels that are C-1 (low concentration), C-2 (medium concentration) and C-3 (high concentration) and measured for kit at the Seoul National University Hospital. Recovery rate is evaluated after measurement at four different days. Results: Recovery rate results using WHO certified reference material are T4 90%, Ferritin 88%, PSA 94%, Prolactin 99%, AFP 94% and TSH 93%. Conclusion: A procedure that appropriate accuracy, precision, specificity, sensitivity, reproducibility, and validate on the subject of kit for radioimmunoassay is essential. Recovery rate assay as extraction efficiency of analysis process is percent about already measuring results of analysis result after all measuring process. This is very important assessment standards of performance evaluation of immunoassay kit. Recovery rate results of 6 type used WHO CRM are satisfactory to 88~99%. This demonstrates that the radioimmunoassay is a very accurate measurement, which is very effectively utilized in clinical practice.

• Proceedings of the Korea Air Pollution Research Association Conference
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• 2004.11a
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• pp.298-299
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• 2004

• Analytical Science and Technology
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• v.22 no.5
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• pp.376-385
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• 2009

In our study, the accuracy for measurement of seventeen 2,3,7,8-substituted PCDDs/PCDFs in certified reference material (CRM) which is the sample of homogeneous sediment matrix taken from an area known to have significant chemical contamination, particularly PCBs (polychlorinated biphenyls), was evaluated. Though the methodology in this study followed the official method of unintentionally produced persistent organic pollutants (UPOPs) announced by the Ministry of Environment of the Republic of Korea in 2007, there were slight changes using additional purification step by activated carbon column because the interferences of sample were not sufficiently removed when only multi-silica column and alumina column have been used for purification. The |En| number proposed by the Korea Research Institute of Standards and Science was used for a valuation basis of the accuracy. The |En| numbers of seventeen 2,3,7,8-substituted PCDDs/PCDFs have been indicated as 1 and below, they were decided "Pass" in this test, when DB-5MS column and SP-2331 column were used together. Because 1,2,3,7,8-PeCDD and #169-HxCB were not separated on DB-5MS column, the ions of 1,2,3,7,8-PeCDD were selected at M/M+2 instead of M+2/M+4 suggested by EPA 1613. It is possible to distinguish them in HRGC/HRMS analysis.

• 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.

• 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.

• 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.

• 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.

• Analytical Science and Technology
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• v.26 no.1
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• pp.91-98
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• 2013

Interested in NOA (Naturally Occurring Asbestos), Korea as well as the USA has been making geologic maps of asbestos distributed mines and surrounding areas, restoring mines, evaluating hazard, and so on. The result can be used to improve the reliability of analysts and analysis institutions by judging the amount of asbestos and set up PLM(Polarizing Light Microscope) information by analyzing in soil. The certification value of 2 kinds of CRM(Certified Reference Material) was performed by counting total 400 points with EPA 600-R-93-116 method using by PLM. The following is the result of homogeneity and stability of 2 kinds of manufactured CRM analyzed by ANOVA (Analysis of variance) and Regression Analysis. Based on the analyzation, the results are satisfied with homogeneity and long-term stability. The analyzed certification value of CRM includes the range of minimum and maximum value of point counting result for chrysotile; low concentration-1% (range, 0.25~3.00), high concentration-4% (range, 2.25~5.50).

• Mass Spectrometry Letters
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• v.14 no.4
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• pp.166-172
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• 2023

The utilization of methyl 2-aminobenzoate as a biocide and pesticide has raised concerns regarding its potential toxicity. To assess its safety, it is crucial to determine its quantity and related toxicity using reference materials (RMs) or certified reference materials (CRMs). As an RM and CRM containing methyl 2-aminobenzoate within a biocidal product matrix is currently unavailable, this study aimed to produce a high-quality RM containing methyl 2-aminobenzoate, ensuring its homogeneity and stability, following the ISO Guide 35 and ISO 17034. The study determined that the produced RM exhibited homogeneity, as indicated by a calculated F-value (1.91) smaller than the critical F-value (3.02). In the assessment of isochronous short-term stability, the slope of the linear regression for the RM showed no statistically significant difference from zero when stored at temperatures of 4, 18, and 60 ℃ for 4 weeks. Regarding classical long-term stability, the RM demonstrated sustained stability over the course of one year when stored at 4 ℃. This study has successfully developed an RM for monitoring methyl 2-aminobenzoate in biocides and pesticides. Its quality underwent rigorous evaluation, confirming both homogeneity and stability.