• Analytical Science and Technology
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• v.23 no.3
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• pp.261-268
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• 2010

This study was performed to evaluate the PCBs-containing wastes using official test method. Ninety samples of transformer oil and various solid waste were collected to assess the analytical results. In the analysis of PCBs-containing wastes, the PCBs levels were detected in the range of 7.6 mg/kg to 23.8 mg/kg for transformer oils, $0.02\sim0.54\;{\mu}g/100cm^2$ for plat solid wastes, and 0.01~0.071 mg/kg for amorphous solid waste. In the cupper wire waste of the transformer with oil concentration level of 23 mg/kg, the analytical result exceed PCBs regulation level of 0.04 mg/kg. The new proposed analytical method for PCBs containing waste can be forced to effective management of the wastes.

• Analytical Science and Technology
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• v.27 no.3
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• pp.167-171
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• 2014

Hydrofluoric acid (HF), a typical inorganic acid, has been used in the industry for its various usage and classified as the toxic compound, because it can cause the pneumonia and pulmonary edema when it was exposed to respiratory organs. The official environmental analytical method for fluorine and its compound in waste has not been developed. For this reason, we have faced some problem to treat the contaminated wastes by the HF leakage from industrial process. In this study, prepared for analytical method for combustible waste (crop, trees, etc.) generated from HF leaking accident and to be applied as the official analytical method for fluorine contaminated waste when the fluorine and its compound will be regulated as a hazardous material by the waste management law later.

• KSBB Journal
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• v.32 no.1
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• pp.54-62
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• 2017

This study aimed to estimate the measurement uncertainty related to determination of hyaluronic acid used as a dietary supplement by high-performance liquid chromatography. According to the guidelines of the Association of Official Analytical Chemists, the analytical processes for determination of hyaluronic acid were performed. And the measurement uncertainty obtained during the analytical processes were expressed in accordance with mathematical/ statistical guidances of GUM (Guide to the Expression of Uncertainty in Measurement) & EURACHEM (Focus for Analytical Chemistry in Europe) for the analytical operations. For the uncertainty in measurement produced based on this analytical method, the expanded uncertainty was calculated by using the relative standard uncertainty between analytical results and sources of uncertainty in measurement (sample weight, final volume, extraction volume, standard solution, matrix and instrument etc). In the results of 95% confidence interval, it was calculated that the uncertainty in measurement was $57.75{\pm}8.76{\mu}g/kg$ (k=2.0). Therefore, it showed that the measurement uncertainty obtained by this analytical method influences on 15.2% of the contents of hyaluronic acid as the analytical results.

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.3
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• pp.342-351
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• 2016

This study was carried out to develop an optimized analytical method using high-performance liquid chromatography (HPLC) applied to canthaxanthin, which is not yet designated as a food colorant in Korea, as well as to perform validation and uncertainty evaluation of this method. Official methods of AOAC, UK, and Japan with HPLC-UV detection were evaluated for the analysis of canthaxanthin by comparison of linearity, resolution, selectivity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, recovery, inter-laboratory tests, and uncertainty measurement. The calibration curves showed high linearity with an $R_2$ value of over 0.999 for canthaxanthin standard solutions in all three official methods. The official method of Japan exhibited the best results in terms of resolution and selectivity, including the lowest LOD and LOQ. The average coefficients of variation were calculated as less than five of three institutes with a precision value less than 1, accuracy near 100%, and recovery ratio between $100{\pm}10%$. The expanded uncertainty for canthaxanthin was estimated to be $39.5{\pm}5.29mg/kg$ (95% confidence level, k=2), and the uncertainty of measurement was 13.4%. In this study, official methods of canthaxanthin were compared and the validities verified. The results will be further applied to establish an authorized analytical method for canthaxanthin in Korea.

• Korean Journal of Environmental Agriculture
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• v.34 no.2
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• pp.111-119
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• 2015

BACKGROUND: Ethychlozate (ECZ) is a plant growth regulator of synthetic auxin for agricultural commodities (ACs). Accurate and sensitive method to determine ECZ in diverse ACs on global official purpose is required to legal residue regulation. As the current official method is confined to the limited type of crops with poor validation, this study was conducted to improve and extend the ECZ method using high-performance liquid chromatography (HPLC) in all the registered crops with method verification. METHODS AND RESULTS: ECZ and its acidic metabolite (ECZA) were both extracted from acidified samples with acetone and briefly purified by dichloromethane partition. ECZ was hydrolyzed to form ECZA and the combined ECZA was finally purified by ion-associated partition including hexane-washing. The instrumental quantitation was performed using HPLC/ FLD under ion-suppression of ECZA with no interference by sample co-extractives. The average recoveries of intra- and inter-day experiment ranged from 82.0 to 105.2% and 81.7 to 102.8%, respectively. The repeatability and reproducibility for intra- and inter-day measurements expressed as a relative standard deviation was less than 8.7% and 7.4%, respectively. CONCLUSION: Established analytical method for ECZ residue in ACs was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

• Analytical Science and Technology
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• v.20 no.2
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• pp.91-108
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• 2007

This study was investigated both the Korean official soil test method and the international various methods for PCBs in soil sample. The analytical guideline of PCBs in contaminated soil were proposed based on the official soil test methods by discussing the extraction, column cleanup, instrumental conditions, quantification methods of peak matching and individual isomers. The total 28 soil samples were selected by consideration of PCBs-contamination, land use etc., and then analyzed using gas chromatography/electron capture detection (GC/ECD) and gas chromatography/mass spectrometry(GC/MS). In this study, the PCBs were not detected as peak matching method using GC/ECD, but PCBs detected $0.002{\sim}0.487{\mu}g/kg$ using GC/MS in background concentrations.

• Journal of Korean Society on Water Environment
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• v.21 no.6
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• pp.549-563
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• 2005

The study was carried out to develop and standardize the analytical method of 1,4-dioxane in water. The National Institute of Environmental Research in Korea has monitored for 1,4-dioxane in water since 1998 and it has been detected in environmental water occasionally. But the environmental pollution and analytical method in water is not well known over the world. The trace analytical method at low-${\mu}/L$ level is prerequisite in order to evaluate the residue of 1,4-dioxane in water. Evaluation of the method was demonstrated by comparing and analyzing with liquid-liquid extraction, solid-phase extraction and purge & trap technique. As a result of experiment by standard solutions and raw samples, the precision and accuracy for three methods were obtained within error rate of about 10%. Therefore, three methods were standardized as official monitoring method in Korea. Also, a convenient and simple liquid-liquid extraction method for the analysis of 1,4-dioxane in water was developed by combined with gas chromatography/mass spectrometry and applied to the water samples in Korea

• Korean Journal of Environmental Agriculture
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• v.14 no.3
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• pp.338-344
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• 1995

The wet ash method has been used as an official standard procedure for the analysis of Cd in brown rice in Korea, but this method involves several disadvantages. Thus, four analytical methods were compared in this experiment in order to find a more efficient method for the Cd analysis in brown rice. Evaluation was made based on both the Cd recovery percentages from the Cd-spiked samples and the relationships between Cd contents obtained by the official procedure and other methods. Results showed that ashing 50g brown rice at $600^{\circ}C$(dry ash method) recovered nearly 80% of the spiked Cd. This recovery percentage was a little lower than that of the wet ash method(87%) but higher than those of other methods. The dry ash method had the lowest standard deviations and revealed the highest correlation coefficient($r=0.98^{\ast\ast}$) in Cd contents with the standard wet ash method. These results demonstrated that the dry ash method, ashing 50g brown rice at $600^{\circ}C$, would be as efficient as the wet ash method and could be employed as a recommended procedure for the Cd analysis of brown rice.

• Analytical Science and Technology
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• v.21 no.3
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• pp.174-182
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• 2008

The study on the development of rapid analytical method of PCBs containing waste was performed by considering the extraction, column cleanup process, analytical condition and so on. In the established method, new sample clean-up procedure, new quantification peaks and temperature program were introduced. Method detection limit of the method was 0.5 mg/L, and the method could save the total run time to 2/3, therefore save the analysis cost, The new rapid analytical method of transformer oil was suggested to the waste official test method.

• Korean Journal of Environmental Agriculture
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• v.39 no.2
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• pp.130-137
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• 2020

BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r²>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.