• Mass Spectrometry Letters
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• v.10 no.4
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• pp.112-116
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• 2019

In this study, a chloroform consumer chemical product (CCP) reference material (RM) is successfully developed, with potential to be used in the proficiency testing of hazardous compounds in CCPs for analysis and testing agencies. Validation experiments are rigorously conducted to evaluate whether the RM meets the requirements set by the ISO 13528 and ISO Guide 35, using a reliable GC/MS method for the analysis of chloroform. The obtained calibration plot linearity, limit of detection (LOD), and limit of quantitation (LOQ) are excellent. The developed RM meets the homogeneity and stability requirements; the between-unit (s_bb) and within-unit (s_wb) standard deviations are less than 2.5%, and the stability is found to be guaranteed for 50 days.

• Journal of Soil and Groundwater Environment
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• v.19 no.6
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• pp.49-58
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• 2014

This study was implemented as a part of the experiment to develop two kinds of soil-based Benzo[a]pyrene (BaP) proficiency testing materials (PTMs) for soil analysis. A test was carried out for the check of solubility of the reference material (high purity reagent) using several solvents. Another test was also conducted for the evaluation of homogeneity and stability of two kinds of candidate soil reference materials. The test analysis of BaP in terms of the candidate materials was conducted according to the Standard Soil Analytical Methods by Ministry of Environment. Dissolution of the reference material was shown to vary depending on solvent type and was higher in the order of Dichloromethane > Acetone > Acetone/MeOH (9 : 1) > N-hexane. In addition, the slope on calibration curve for BaP standard solutions was largest on BaP standard solutions prepared with dichloromethane of the tested solvents. Such tendency appeared egually in the commercial BaP standard solution. Therefore, it is thought to be reasonable to use dichloromethane as the solvent in case of the standard stock solution that is used for the measurement of BaP concentration in soil. ISO 13528 and IUPAC protocol were used for verification of homogeneity on the two kinds of soil candidate materials, Both candidate materials were sufficiently homogeneous. Stability assessment of the two candidate materials was made according to ISO Guide 35 and the result showed that both batches did not have any long-term and short term stability issues that might occur during shipping. However, monitoring results of BaP concentration in soil showed that BaP concentration of the two batches measured at 15 days after the sample preparation was reduced by about 24~37% compared with that of the samples measured on 0 day of the sample preparation. Identification was done with several treatments such as irradiation and sterilization etc. The major cause was shown to be irradiation to the samples.

• The Korean Journal of Pesticide Science
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• v.20 no.3
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• pp.211-220
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• 2016

This study was to develop the analytical reference material of green-pepper for multi-residue analysis of pesticides. According to the ISO Guide 35, ISO Guide 13528 and EURL-PT protocol, the homogeneity, stability, assigned value and uncertainty were calculated to assess if it was suitable to be used as the proficiency test or quality control. The values of the within-bottle standard variation ($s_{wb}$) and the between-bottle standard variation ($s_{bb}$) were 1.7~3.7% of assigned value according to the requirement of the ISO guide 35. And, the uncertainty ($u^*{_{bb}}$) due to inhomogeneity was 0.8~1.1% for all pesticides. The storage stabilities of ten-pesticides at various conditions were assessed. For all target pesticides, the slop ($b_1$) values were smaller than the corresponding values of $[t_{0.95,n-2}{\times}s(b_1)]$ specified by the ISO guide 35, indicating that there were no statistically significant decreases in the concentration of the target pesticides when the analytical reference material was stored at room temperature ($20{\sim}30^{\circ}C$) for 7 days, freezing ($-20^{\circ}C$) for 30 days and deep freezer ($-80^{\circ}C$. except for bifenthrin, fenpropathrin) for 245 days. For proficiency test by using it developed by Korea Institute of Toxicology, inter-lab test was performed with eight organization performing the residual pesticide analysis. We found that there were some different results among them. Some were assessed as questionable or unacceptable for two pesticides and one organization didn't analyze the six pesticides. From these results, this green-pepper analytical reference material containing ten-pesticides could be used as a tool for the proficiency test to improve the reliability or consistency for pesticide residue's results.

• Analytical Science and Technology
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• v.23 no.5
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• pp.485-491
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• 2010

A certified reference material (CRM) of KRISS 109-03-SSD was developed for the analysis of hazardous elements in soil. The target elements were As, Cd, Cr, Cu, Hg, Ni, Pb, Zn being regulated by the Soil Environment Conservation Act. Starting material was collected from tailing dump of an unworked tungsten mine at Sangdong (Gangwon-do, Korea). The starting material under-went through a series of fabricating process steps of screening, drying, grinding, sieving, blending, bottling, sterilization and was certified according to the ISO Guide 35. Isotope dilution-inductively coupled mass spectrometry (ID-ICP/MS) and instrumental neutron activation analysis (INAA) were used for the measurement. Homogeneity was tested according to ISO 13528 annex B. The certified values were determined using the results from two different methods or from two independent measurements using a method. Finally, certified values of seven elements of arsenic, cadmium, chromium, copper, lead, nickel and zinc were determined. Mercury did not satisfied the criteria of homogeneity and the result would be provided for information only, together with iron and tungsten. It was also studied, the extractable fraction of elements by aqua regia according to the ISO 11466 protocol being frequently studied for the purpose of environmental monitoring. It was performed as a inter-laboratory study by 6 laboratories of a public institute and universities. Standard deviation among the laboratories was much bigger than the uncertainty of the certified value. The result of inter-laboratory study on the extractable fraction will be provided for information, only.

• Journal of Soil and Groundwater Environment
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• v.18 no.5
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• pp.15-25
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• 2013

In this study, two kinds of soil-based proficiency testing materials (PTMs), NICE-012L and NICE-012R were prepared and certified for Benzen, Toluene, Etylbenzene and Xylene with evaluation of uncertainties. In order to analyse BTEX (Benzen Toluene Etylbenzene Xylene) for the candidate materials, GC/MS was used after pretreatment according to methods of soil analysis by Ministry of Environment. For the homogeneity test among bottles in terms of candidate materials, ISO 13528 and IUPAC Protocol were used and according to the result, both candidate materials showed sufficient homogeneity. Also, the stability test over the candidate materials was accessed according to the ISO Guide 35 by classifying short-term and long-term stability and the result showed that both candidate materials showed decent stability. The reference values of the two candidate materials depending on BTEX components were derived from the average of the 11 samples that were used for verification of the samples' homogeneity. Uncertainty of measurement was combined by uchar that was caused by a characteristic value, $u_{bb}$ that was caused by between-bottle homogeneity, and $u_{stab}$ that was caused by stability, and then combined uncertainty ($u_{PTM}$) was multiplied to the coverage factor (k) derived from the effective degree of freedom from each factor that leads to expanded uncertainty (U) in about 95% of confidence level. The proficiency testing materials developed through this study were supplied to National Institute of Environmental Research (NIER) and utilized as an external proficiency testing materials for evaluating analysis capacity of soil agencies with specialty in terms of soil analysis approved by Minister of Environment.

• Korean Journal of Environmental Agriculture
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• v.35 no.3
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• pp.223-233
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• 2016

BACKGROUND: This study was to develop a analytical reference material including twenty pesticides in tomato. To use it for proficiency test, the suitability of homogeneity, storage stability, assigned values and uncertainty for analytical reference material were important.METHODS AND RESULTS: In order to develop a analytical reference material of tomato for multi-residue analysis of pesticides, twenty-pesticides were treated in tomato and the samples were frozen and homogenized. The homogeneity, stability, assigned value and uncertainty were calculated according to the requirements of the KS A ISO Guide 35, KS Q ISO 13528 and EURL-PT protocol. The values of the within-bottle standard variation(s_wb) and the between-bottle standard variation(s_bb) were 0.9~6.5% of assigned value and the uncertainty(u*_bb) due to inhomogeneity was also calculated as 0.6~1.9% for all pesticides. This indicated that it was satisfactory to be used as a analytical reference material. The storage stabilities of twenty-pesticides at room temperature and freezing conditions were assessed according to the requirement of the KS Q ISO Guide 35. All pesticides were stable at room temperature (20~30℃) for 8 days and freezing (-20℃) for 23 days.CONCLUSION: The feasibility of analytical reference material for pesticide multi-residue analysis in a tomato matrix was investigated. Homogeneity of within/between-bottle, uncertainty and stabilities at room temperature and freezing condition were satisfactory for a use of proficiency test and quality control. From these results, a analytical reference material would be applicable to monitor the proficiency test of pesticide analysis organizations to improve the reliability and consistency.