• Journal of Biosystems Engineering
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• v.34 no.5
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• pp.371-376
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• 2009

Microwave digestion is a preferred pretreatment method for agricultural samples because of its quick chemical reaction and minimum loss of analytes. In this research, a feedback temperature controller was developed to control the temperature inside a vessel for the microwave-assisted digestion system. An existing industrial microwave oven was fitted with the temperature controller for controlling inside temperature of the vessel. Four control methods, On/Off, proportional (P), proportional integral (PI), and proportional integral derivative (PID) were used and compared. Experimental results showed that PID control produced best temperature control performance. The PID controller could maintain the temperature of water sample and rice sample in the digestion system with error range of $-2.5{\sim}3.3^{\circ}C$ and $-1.9{\sim}0.5^{\circ}C$ at set temperature of $170^{\circ}C$, respectively.

• Bulletin of the Korean Chemical Society
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• v.15 no.9
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• pp.786-791
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• 1994

A simple and rapid sample pretreatment process necessary for determination of metal oxides in water was proposed. Samples were injected into the continuous-flow tube installed inside the microwave oven and the treated samples were cooled before entered to the Ion Chromatography (IC) or Inductively Coupled Plasma (ICP). By coupling this microwave digestion system with IC or ICP, a fully automatic analytical procedures may be easily established. In this study, two different types of digestion methods were considered; the open tubing method (OTM) and the restraint tubing method (RTM). The RTM was proved to be 3 times faster in digestion period and 10 times higher in detection range than the OTM. Validation of proposed sample digestion system was carried out by using an ICP. The results showed that both of continuous-flow methods, the OTM and the RTM were comparable in accuracies with the conventional batch-type vessel digestion method.

• Analytical Science and Technology
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• v.14 no.4
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• pp.324-330
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• 2001

For the analysis of S, P and Zn in lubricating oil, microwave digestion method was studied by using inductively coupled plasma-atomic emission spectrometry(ICP-AES). Lubricating oil was completely decomposed with nitric acid or a mixture of nitric acid and hydrogen peroxide using and closed microwave digestion system. Digestions are completed within 50 min, a factor of at least 3~4 times faster than for the conventional digestion. A gradual heating program operated by the pulsed mode was found suitable for decomposing the lubricating oil matrix safely. The proposed method of digestion gave relative standard deviations(RSD) less than 3% for the elements determined.

• Journal of Radiation Protection and Research
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• v.37 no.4
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• pp.213-218
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• 2012

Alpha spectrometry has been typically used for determination of the uranium isotopes in soil. For a number of uranium analysis in soil samples, rapid sample digestion with limited quantities of mixed acid containing HF will give a contribution for effective management of uranium analysis. Microwave digestion system is evaluated for rapid sample digestion using reference uranium soil (IAEA-375 soil). For completion of 0.5 g of soil digestion by microwave, 3 ml of HF in a 10 ml of mixed acid is minimum requirement volume for completed soil digestion for 80 minutes. Microwave digestion is timely effective techniques for uranium measurement using alpha spectrometry compared to the other methods (open vessel digestion, closed vessel digestion) due to rapid sample digestion. In addition, it can be reduced the occurrence of hazardous substances by minimizing the amount of HF.

• 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.

• 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.

• 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.

• 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 Technical Association of The Pulp and Paper Industry
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• v.43 no.1
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• pp.65-73
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• 2011

The fibrous raw materials in packaging-grade paper production in Korea were mainly obtained from waste paper. The use of recycled paper has both positive and negative impacts in papermaking process. The primary positive impacts are the environmental protection and manufacturing cost reduction, and the negative impacts are the quality reduction in paper quality and the accumulation of heavy metals and other pollutants in wet- and dry-end process. This study was carried out to consider the optimum acid decomposition system with the highest recovery rate for the analysis of heavy metals in packaging-grade paper. The open digestion system using Kjeldahl apparatus and the closed digestion system using microwave oven for decomposing the organic materials in paper were compared. In both open and closed digestion method, the combination of nitric acid, hydrochloric acid and hydrogen peroxide showed higher recovery rate than using only nitric acid alone because the presence of Cl- ions in hydrochloric acid stabilizes ligand formation with metal ions. KOCC was observed to have the highest heavy metal content among the recycled paper samples. The heavy metal contents decomposed with the closed digestion system were relatively higher than with open digestion system.

• 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.