• Korean Journal of Veterinary Research
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• v.52 no.2
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• pp.69-74
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• 2012

The analytical method of trace toxic metals in livestock products was confirmed and validated through certified reference material (CRM) and the international proficiency tests. There are some difficulties to determine low levels of toxic metals in livestock products because of interferences due to the matrix. The recoveries of CRM (NIST 1577c) ranged from 73.9 to 119% for lead and from 86.4 to 111% for cadmium in bovine liver. The international proficiency tests were carried out with the milk powder and cocoa powder samples including metals provided by Food Analysis Performance Assessment Scheme (FAPAS$^{(R)}$, UK). The test samples were prepared by microwave digestion using solution of $HNO_3:H_2O_2:H_2O$ (v/v/v = 5 : 2 : 4) and analyzed by ICP/MS. The analytical result of cadmium in milk powder was $121{\mu}g/kg$ with -0.3 of the z-score compared to the assigned value of $131{\mu}g/kg$ by FAPAS$^{(R)}$. The analytical results of lead and cadmium in cocoa powder were $29.2{\mu}g/kg$ and $97.6{\mu}g/kg$, respectively, which satisfied the assigned values of $34.2{\mu}g/kg$ for lead and $126{\mu}g/kg$ for cadmium by FAPAS$^{(R)}$. It is verified that the analytical method is accurate and reliable to determine trace lead and cadmium in livestock products by microwave digestion and ICP/MS.

• Journal of Radiation Protection and Research
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• v.41 no.4
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• pp.359-367
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• 2016

Background: As new legislation has come into force implementing radiation safety management for the use of naturally occurring radioactive materials (NORM), it is necessary to establish a rapid and accurate measurement technique. Measurement of $^{238}U$ and $^{232}Th$ using conventional methods encounter the most significant difficulties for pretreatment (e.g., purification, speciation, and dilution/enrichment) or require time-consuming processes. Therefore, in this study, the applicability of ED-XRF as a non-destructive and rapid screening method was validated for raw materials and by-product samples. Materials and Methods: A series of experiments was conducted to test the applicability for rapid screening of XRF measurement to determine activity of $^{238}U$ and $^{232}Th$ based on certified reference materials (e.g., soil, rock, phosphorus rock, bauxite, zircon, and coal ash) and NORM samples commercially used in Korea. Statistical methods were used to compare the analytical results of ED-XRF to those of certified values of certified reference materials (CRM) and inductively coupled plasma mass spectrometry (ICP-MS). Results and Discussion: Results of the XRF measurement for $^{238}U$ and $^{232}Th$ showed under 20% relative error and standard deviation. The results of the U-test were statistically significant except for the case of U in coal fly ash samples. In addition, analytical results of $^{238}U$ and $^{232}Th$ in the raw material and by-product samples using XRF and the analytical results of those using ICP-MS ($R^2{\geq}0.95$) were consistent with each other. Thus, the analytical results rapidly derived using ED-XRF were fairly reliable. Conclusion: Based on the validation results, it can be concluded that the ED-XRF analysis may be applied to rapid screening of radioactivities ($^{238}U$ and $^{232}Th$) in NORM samples.

• The Korean Journal of Nuclear Medicine Technology
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• v.15 no.2
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• pp.116-124
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• 2011

Purpose: To establish accurate external quality assurance (EQA) test, cross institutional and modality tests were performed using WHO certificated reference material (CRM) and same pooled patients serum. Materials and Methods: Accuracy and precision were evaluated using CRM and pooled patients' serum for AFP, CEA, PSA, CA 125, CA 19-9, T3, T4, Tg, TSH. To evaluate the accuracy and precision, recover test and coefficient variation were measured. RIA test were performed in major 5 RIA laboratory and EIA (CLIA) test were done in 5 major EIA laboratory. same sample of CRM and pooled serum were delivered to each laboratory. Results: In 2009, mean precision of total tumor marker of RIA was $14.8{\pm}4.2%$ and that of EIA(CLIA) was $19.2{\pm}6.9%$. In 2010, mean precision of 5 tumor marker and T3, T4, Tg, TSH was $13.8{\pm}6.1%$ in RIA and $15.5{\pm}7.7%$ in EIA (CLIA). There was no significant difference between RIA and EIA. In RIA, the coefficient variations (CV) of AFP, CEA, PSA, CA 125, T3, T4, TSH were within 20%. The CV of CA 19-9 was over 20% but there was no significant difference with EIA (CLIA) (p=0.345). In recovery test using CRM, AFP, PSA, T4, TSH showed 92~103% of recovery in RIA. In recovery test using commercial material, CEA, CA 125, CA 19-9 showed relatively lower recovery than CRM but there was no significant difference between RIA and EIA (CLIA). Conclusion: By evaluating the precision and accuracy of each test, EQA test could more accurately measured the quality of each test and performance of laboratory.

• Mass Spectrometry Letters
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• v.3 no.2
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• pp.54-57
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• 2012

Mass spectrometric analysis was carried out using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) for the precise and accurate determination of the isotope ratios of ultratrace levels of uranium dissolved in 3% $HNO_3$. We used the certified reference material (CRM) 112-A at a trace level of 100 pg/mL for the uranium isotopic measurement. Multiple collectors were utilized for the simultaneous measurement of uranium isotopes to reduce the signal uncertainty due to variations in the ion beam intensity over time. Mass bias correction was applied to the measured U isotopes to improve the precision and accuracy. Furthermore, elemental standard solution with certified values of platinum, iridium, gold, and thallium dissolved in 3% $HNO_3$ were analyzed to investigate the formation rates of the polyatomic ions of $Ir^{40}$ $Ar^+$, $Pt^{40}$ $Ar^+$, $Tl^{40}$ $Ar^+$, $Au^{40}$ $Ar^+$ for the concentration range of 50-400 pg/mL. Those polyatomic ions have mass-to-charge ratios in the 230-245 m/z region that it would contribute to the increase of background intensity of uranium, thorium, plutonium, and americium isotopes. The effect of the polyatomic ion interference on uranium isotope measurement has been estimated.

• Korean Journal of Agricultural Science
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• v.46 no.2
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• pp.315-322
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• 2019

In this study, the contents of ${\beta}$-carotene and cholesterol were evaluated in various types of agricultural and processed foods (vegetables, legume products, dairy products, and eggs). Certified reference material (CRM) with an assigned value was used for the validation of the ${\beta}$-carotene and cholesterol analytical methods. High recoveries (accuracy) of ${\beta}$-carotene (96%) and cholesterol (97%) were obtained from the quantitative analysis of the CRM, with a relative standard deviation (%) of 1.86 and 3.35% for the ${\beta}$-carotene and cholesterol, respectively. Vegetables contained relatively high concentrations of ${\beta}$-carotene (raw Toona sinensis, $1650.97{\mu}g/100g$, a raw small onion, $879.09{\mu}g/100g$, and a raw lettuce stem, $591.89{\mu}g/100g$). The ${\beta}$-carotene values in dried chickpeas ($22.94{\mu}g/100g$) and dried brown lentils ($21.98{\mu}g/100g$) were similar. The highest ${\beta}$-carotene value among the analyzed dairy products was found in banana milk ($234.21{\mu}g/100g$) while other flavored products (strawberry milk and chocolate milk) did not contain any ${\beta}$-carotene. Furthermore, ${\beta}$-carotene was not detected in goat milk and high calcium milk in this study. With regard to cholesterol among the analyzed samples, the highest cholesterol value was found in egg yolk (629.30 mg/100 g), and cooking methods (boiling and frying) had little effect on the cholesterol levels of eggs. In addition, the cholesterol content in vanilla ice cream was 28.77 mg/100 g which was the highest value among the analyzed dairy products.

• Journal of Radiation Protection and Research
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• v.36 no.4
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• pp.223-229
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• 2011

Ba is the most useful element to get the $Ba(Ra)SO_4$ precipitate. However, when the high concentrations of ions such as sulfate, calcium are existed in the leachate of phosphogypsum stack, it is difficult to get the $Ba(Ra)SO_4$ precipitate. Since this reason, the developed method for the Ba coprecipitate using EDTA was performed to determine the $^{226}Ra$ concentration in the high sulfate sample. The average concentration of $^{226}Ra$ in a leachate of phosphogypsum using this method was 0.102 $Bq{\cdot}kg^{-1}$ and the minimal detectable activity is 3.4 $mBq{\cdot}kg^{-1}$. The $mBq{\cdot}kg^{-1}$ method was 0.102 $Bq{\cdot}kg^{-1}$ and the minimal detectable activity is 3.4 $mBq{\cdot}kg^{-1}$. The $^{226}Ra$ stock solution and the CRM (Certified Reference Material) were analyzed to verify this method. In analyzed $^{226}Ra$ stock solution, bias with added concentration was approximately 1% and the correlation curve between $^{226}Ra$ concentration in simulated standard sample and measured $^{226}Ra$ concentration showed good agreement with a correlation coefficient ($R^2$) of 0.99. In analyzed CRM, maximum bias with reference value was 5.8% (k=1) and the analytical results were in good agreement with the reference value.

• Analytical Science and Technology
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• v.21 no.4
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• pp.316-325
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• 2008

An inductively coupled plasma mass spectrometry (ICP-MS) instrument equipped with flow injection-hydride generation system was used for the determination of trace arsenic in seawater sample. The accuracy in this method was verified by the analysis of certified reference materials (CRM) of seawater (CASS-4, NASS-5). The analytical results agreed with certified value within the range of uncertainty. The expanded uncertainties for CASS-4 and NASS-5 in this experiment were ranged from 6.2% to 6.8% obtained from repeated analyses of the CRMs (n=5). The detection limit of $As^+$ (m/z=74.9216) in this method was confirmed about 0.01 ug/kg. Linearity obtained from calibration curve of arsenic was excellent ($R^2=1$). The detection at $As^+$ (m/z=74.9216) and $AsO^+$ (m/z=90.9165) by using oxygen reaction gas in DRC mode was compared. Sensitivity at $AsO^+$ (m/z=90.9165) was decreased about 25-fold, but the analytical results are the same that at $As^+$ (m/z=74.9216).

• Journal of the Society of Disaster Information
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• v.9 no.3
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• pp.249-258
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• 2013

Recieved Mar. 06, 2013 Revised Mar. 29, 2013 Accepted Sep. 11, 2013In this study, we evaluated the method performance and the optimum sample injection method of the portable GC/MS(HAPSITE) which were designed to operate on scene of chemical accidents. Chemicals used for performance test were vinyl chloride(VC), methyl chloride(MC), benzene(Bz), toluene(Tol). CRM(Certified Reference Material) Manufactured by KRISS(Korea Research Institute of Standards and Science) was used as the standard gas. The results showed that 1) Among three sample injection methods(Cylinder, Silico canister, and Bag), bag was identified as the most appropriate sample injection method. Bag material and capacity did not significantly affect the results. The most ideal reproducibility occurred at the 2-minute point of the purge time in the loop and tenax methods. 2) Performance evaluation of HAPSITE was conducted. Evaluation items were reproducibility, linearity, method detection limit, etc. Tenax concentration method was appropriate for larger molecules and Carbopack concentration method was suitable for smaller molecules.

• Korean Journal of Food Science and Technology
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• v.37 no.3
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• pp.352-359
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• 2005

Uncertainty involved during determination of vitamin C content in infant formula was quantified by indophenol titration method. Uncertainty sources in measurand, such as purity, weight, final volume of standard, volume of standard solution used for titration, sample weight, final volume of sample, extraction solution used for titration, titration of extraction solution and standard solution by indophenol solution were identified and used as parameters for combined standard uncertainty based on Guide to the expression of uncertainty in measurement (GUM) and Draft EURACHEM/CITAC Guide. Uncertainty parameters of each source in measurand were identified as resolution, reproducibility and stability of chemical balance, standard material purity, repeatability, reproducibility, end point of titration, 1 mL pipet, 5 mL autopipet, and 100 mL mass flask. Each uncertainty component was evaluated by types A and B and included to calculate combined uncertainty. Analytical test result for traceability under laboratorial conditions using Certified Reference Material (CRM) test was certified as $108.4{\pm}1.7mg/100g$, which was within CRM certification range of $114.6{\pm}6.6mg/100g$. Uncertainty test result of vitamin C content of 5 g sampling was $56.7{\pm}2.44mg/100g$. Uncertainty could be reduced by identification of uncertainty sources and components related with vitamin C determination by indophenol titration method and by decreasing uncertainty sources and components.

• Analytical Science and Technology
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• v.21 no.4
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• pp.284-295
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• 2008

For plastics samples, a method using combustion ion chromatography was selected as a method for rapid low-cost analysis to test whether hazardous substances are contained or not. Using combustion ion chromatography, a verification test for F, Cl and Br compounds generated a linear calibration curve with a correlation coefficient of $r^2$ = 0.999~1.000 in the calibration range from 0.5 to 4.0 mg/kg. The detection limits were found to be 0.005~0.024 mg/kg and quantitative limits were found to be 0.014~0.073 mg/kg. The recoveries of combustion ion chromatography using certified reference material (CRM) were found to be 95.5~104.9%. Based on these results, a proficiency test was conducted together with several laboratories in and out of the country, to make comparative analysis of the results from each laboratory. As a result, the data supported the use of combustion ion chromatography as an effective analysis method to deal with regulations for halogen-free electronic products and for other hazardous substances in the electronic products.