• Analytical Science and Technology
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• v.16 no.3
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• pp.212-217
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• 2003

The memory effect of silver and aqua regia in the vessel by their permeation was studied during the microwave digestion of samples under the operating conditions of high temperature and pressure. The extent of permeation in vessels with the solution containing silver 5 mg has been shown to be $0.97{\mu}g/mL$ for the digestion of $HNO_3$ solution and $0.47{\mu}g/mL$ for the digestion of oil sample under condition of MDS 180T program ($180^{\circ}C$, 220 psi).

• Proceedings of the Korean Environmental Health Society Conference
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• 2002.04a
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• pp.16-19
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• 2002

This study was carried out to establish the standardized analysis method in order to decide accurate concentrations of hazardous metals in the air. Acid decomposition method used usually was compared to microwave digestion method. Comparing results of tested background concentration in blank filter, we found that the magnitude of element concentration was Na, Ca, K, Mg, Al and Ba by order. The element concentrations of Glass fiber filter were higher than those of Quartz fiber filter, and the number of undetected components in Glass fiber filter was lower than that in Quartz fiber filter. Thus it is supposed that the concentration of background elements in Glass fiber filter was higher than those in Quartz fiber filter The extraction rate of microwave digestion method was superior to those of acid decomposition method during the test of blank filter as well as SRM of NIST. In case of the SRM of NIST, the average extraction efficiency of acid decomposition Method and microwave pretreatment is 53.8∼82.7％, 81.3∼97.1％, respectively. This result might be caused by the closed system of Microwave, which make outflow and loss of components less. Also microwave digestion method has other merits such as the minimization of time, reagents, and contamination. Furthermore, if the extraction condition, extraction time and used acids are optimized, the better results will be represented.

• Proceedings of the Korean Radioactive Waste Society Conference
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• 2004.06a
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• pp.158-166
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• 2004

The optimal conditions are obtained for the decomposition of solid radioactive wastes, including ion exchange resin, zeolite, active charcoal, and sludge from nuclear power plant. In the process of decomposing the radioactive wastes were used the microwave acid digestion method with mixed acid. The solution after acid digestion by the following method was colorless and transparent. Each solution was analyzed with ICP-AES and AAS and the recovery yield for 5 different elements added the simulated radioactive wastes were over 94%. As an effective pre-treatment, the proposed microwave acid digestion conditions concerning the chemical trait of each radioactive waste are expected to be generally applied to above-mentioned radioactive wastes from nuclear power plant hereafter.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.2 no.4
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• pp.231-238
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• 2004

The conditions are obtained for the decomposition of solid radioactive wastes, including ion exchange resin, zeolite, charcoal, and sludge from nuclear power plant. In the process of decomposing the radioactive wastes was used the microwave acid digestion method with mixed acid. The solution after acid digestion by the following method was colorless and transparent. Each solution was analyzed with ICP-AES and AAS and the recovery yield for 5 different elements added into the simulated radioactive wastes were over $94{\%}$. The elemental analysis of destructive low and medium level radioactive wastes by the proposed microwave acid digestion conditions concerning the chemical characteristics of each radioactive waste are expected to be useful basic data for development of optimal glass formulation.

• Journal of the Korean Chemical Society
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• v.38 no.8
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• pp.576-584
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• 1994

The method described offers rapid and efficient sample preparation using on-line microwave digestion of metal oxides in water sample with direct elemental detection by ICP-AES. The open tubing digestion system(OTD) and the restraint tubing digestion system(RTD) for flow injection(FI) were designed and tested to find the optimum conditions. Comparison of OTD and RTD indicated that RTD was 3 times faster on the digestion time, and 10 times higher on sample mass. Finally, the results of RTD agree well with those by conventional microwave open vessel in all cases and show good precision; Fe and Cu show good with about 5% of RSD, while Zn and Co more or less than 10% RSD.

• Applied Chemistry for Engineering
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• v.10 no.4
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• pp.568-575
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• 1999

Two different digestion procedures for the simultaneous determination of major and platinum-group element(PGE) in spent automobile catalysts containing PGE and silicates by inductively coupled plasma atomic emission spectrometry(ICP-AES) are compared. Combinations of mixed aids using HF, $HNO_3$, HCl, $HClO_4$, $H_2O_2$, and $H_3BO_3$ are utilized for the hot plate dissolution method and the closed-vessel microwave digestion method, The latter method has been shown to be relatively superior in terms of recovery, analysis time, and amount of aqua regia (3 parts HCl + part $HNO_3$ required to dissolve PGE in comparison with conventional open vessel hot-plate dissolution. The best results were drawn from the following conditions: In closed Teflon PFA vessels under microwave heating with temperature/pressure regulation, a 0.25 g portion of sample was digested in 2 mL of HF, 2 mL of $HNO_3$ and 6mL of HCl under the pressure of 200 psi(13.79 bar) at $180^{\circ}C$ for 1hr, followed by a second digestion stage with 16 mL of 5%(w/v) boric acid under the pressure of 20 psi(1.38 bar) at $100^{\circ}C$ for 10 min. After the microwave heating, the sample was post-treated with 10 mL of aqua regia twice by hot-plate heating. This condition gives the PGE recovery within 85~110% and the relative standard deviations within 2%. The method developed can therefore be regarded as an alternative method for routine analysis of spent automobile catalysts.

• Korean Journal of Veterinary Research
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• v.43 no.3
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• pp.393-398
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• 2003

Simple and rapid sample preparation method for trace elements in foods of animal origin using ultra high pressure microwave digestion system (UHP/MDS) and inductively coupled plasma atomic emission spectrometer (ICP/AES) were developed. 1. For the digestion of sample using UHP-MDS, 20% nitric acid (v/v) was the most suitable solvent for the determination of trace elements in foods of animal origin. 2. The optimal digestion conditions for UHP-MDS were as follows: final temperature $180^{\circ}C$, final pressure 400 PSI, and magnetic power 900 W in the solid sample. For the liquid sample final temperature $170^{\circ}C$, final pressure 300 PSI and magnetic power 700 W were optimal conditions. 3. As result of interlaboratory test, the average recovery rate of the for solid sample were 88.3~99.1% for As, 82.4~93.3% for Cd, 89.2~101.2% for Hg and 86.5~93.8% for Pb, respectively. In liquid sample, it were 87.0~96.8% for As, 80.9~96.6% for Cd, 87.5~91.2% for Hg and 91.4~95.5% for Pb, respectively. 4. The average coefficient variation rate were 3.3~15.9% for solid sample and 2.9~10.8% for liquid sample.

• Analytical Science and Technology
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• v.23 no.6
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• pp.511-517
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• 2010

Dissolution procedure of vanadium pentoxide, which is widely used as a catalyst for production of sulfuric acid or an oxide reaction of the numerous organic compounds, was investigated. Reagent of vanadium pentoxide was completely dissolved in aqua regia-$H_2O_2$-HF solution, but plate type of vanadium pentoxide sample was not clearly dissolved with mixed acids. Thus, in order to establish the dissolution procedure for plate type of vanadium pentoxide, the solubility of vanadium pentoxide was investigated through comparison of acid treatment-fusion and microwave digestion methods. The optimized acid for dissolution of vanadium compound was found to be mixing acids of aqua regia, $H_2O_2$ and HF. Acid-fusion and microwave digestion methods have a similar property in the solubility of vanadium compound, but the latter was more quick and convenient procedure. The content of vanadium pentoxide was found to be $97.9{\pm}0.9%$ using an inductively coupled plasma atomic emission spectrometer after dissolution of a sample with the microwave digestion system.

• Journal of Korea Society of Waste Management
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• v.35 no.7
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• pp.616-626
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• 2018

The quality standards of solid refuse fuel (SRF) define the values for 12 physico-chemical properties, including moisture, lower heating value, and metal compounds, according to Article 20 of the Enforcement Rules of the Act on Resource Saving and Recycling Promotion. These parameters are evaluated via various SRF Quality Test Methods, but problems related to the heavy metal content have been observed in the microwave acid digestion method. Therefore, these methods and their applicability need improvement. In this study, the appropriate testing conditions were derived by varying the parameters of microwave acid digestion, such as microwave power and pre-treatment time. The pre-treatment of SRF as a function of the microwave power revealed an incomplete decomposition of the sample at 600 W, and the heavy metal content analysis was difficult to perform under 9 mL of nitric acid and 3 mL of hydrochloric acid. The experiments with the reference materials under nitric acid at 600 W lasted 30 minutes, and 1,000 W for 20 or 30 minutes were considered optimal conditions. The results confirmed that a mixture of SRF and an acid would take about 20 minutes to reach $180^{\circ}C$, requiring at least 30 minutes of pre-treatment. The accuracy was within 30% of the standard deviation, with a precision of 70 ~ 130% of the heavy metal recovery rate. By applying these conditions to SRF, the results for each condition were not significantly different and the heavy metal standards for As, Pb, Cd, and Cr were satisfied.

• Mass Spectrometry Letters
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• v.8 no.3
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• pp.53-58
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• 2017

Glycated hemoglobin ($HbA_{1c}$) has been commonly used to screen and diagnose for patients with diabetes mellitus. Here the accelerated procedure of microwave-assisted sample treatment from acid hydrolysis to enzyme digestion followed by isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) was optimized and applied to measure $HbA_{1c}$ in an effort to speed up analysis time. First, two signature peptides of $HbA_{1c}$ and hemoglobin $A_0$ were certified with amino acid analysis by setting optimized acid hydrolysis conditions to $150^{\circ}C$, 1.5 h and $10{\mu}M$ sample concentration in 8 M hydrochloric acid. Consequently, the accurate certified peptides above were used as calibration standards to implement the proteolytic procedure with endoproteinase Glu-C at $37^{\circ}C$, 700 W for 6 h. Compared to the traditional method, the microwave heating not only shortened dramatically sample preparation time, but also afforded comparable recovery yields. The optimized protocol and analytical conditions in this study are suitable for a primary reference method of $HbA_{1c}$ quantification with full SI-traceability and other similar proteins in complex biological samples.