• Korean Journal of Soil Science and Fertilizer
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• v.31 no.3
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• pp.253-258
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• 1998

To verify the suitability of microwave digestion method for analyzing macro nutrients and metals. K, Ca, Mg, Cu, Zn, and Mn contents in plant and composts were investigated comparing with conventional wet digestion method. Because it takes short time to digest metal samples by using microwave method compared with conventional wet digestion method. Digestion time for metal samples was four to six hours long for wet digestion, while one hour long for microwave digestion. Determinant coefficients of Cu, Mn, Zn, Ca, K, and Mg contents between two analyzing methods were 0.99, 0.99, 0.94. 0.97, 0.98, and 0.91, respectively. In the case of Ca and K, microwave digestion method analyzed their contents relatively low compared with wet digestion method. Meanwhile, microwave digestion method analyzed the contents for Cu, Ma, and Zn relatively high compared with wet digestion method. This study results in that microwave digestion method could be an alternative to replacing conventional wet digestion method.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.11 no.1
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• pp.48-55
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• 2001

The purpose of this study was to evaluate the analytical accuracy and precision of microwave oven digestion/atomi absorption spectrophotometry (AAS) for analyzing airborne chromium collected on mixed cellulose ester membrane (M filter from the work environment, and to compare the accuracy and the precision with those of the National Institute for Occupational Safety and Health (NIOSH) Method #7024 hot plate digestion/AAS method. For this study, field air sample pairs were collected from a electroplating process, and spiked samples in a laboratory were prepared and using these samples. Two digestion methods were comp; and evaluated in terms of recovery rate and bias as indices of accuracy and coefficient of variation as a index of precision. The results and conclusions are as follows. In spiked samples, the accuracies (% mean recoveries) of hot plate/AAS and microwave oven/AAS method were 97.19%, 97.1%, respectively, and the precisions (pooled respectively, and the precisions (pooled coefficient of variance, $CV_{pooled}$) 6.93% and 3.88%, respectively. The biases of hot plate ani microwave oven methods were 4.56 - 14.7% and 2.22 - 7.42% respectively. There was no statistically significant difference between hot plate and microwave oven methods recovery rates of spiked samples (p>0,05). Also, no statistically significant difference was shown among the concentrations of air samples determined by two method (p>0.05). In conclusion, microwave oven/AAS method h excellent accuracy and precision, and advantages such as time-saving and simple procedure in comparison with the classical NIOSH method. Therefore, this method can be use widely to analyze airborne chromium collected on MCE filter from the work environments.

• 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 the Korean Chemical Society
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• v.43 no.4
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• pp.412-417
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• 1999

The analytical results obtained by microwave digestion and acid digestion methods for sample pretreatment to determine metal impurities in silicon wafer by inductively coupled plasma-mass spectrometry (ICP-MS) were compared. In order to decompose the silicon wafer, a mixed solution of $HNO_3$ and HF was added to the sample and the metal elements were determined after removing the silicon matrix by evaporating silicon in the form of Si-F. The recovery percentages of Ni,Cr and Fe were found to be 95∼106% for both microwave digestion and acid digestion methods. The recovery percentage of Cu obtained by the acid digestion method was higher than that obtained by the microwave digestion method. For Zn, however, the microwave digestion method gave better result than the acid digestion method. Fe was added to a silicon wafer using a spin coater. The concentration of Fe in this sample was determined by lCP-MS, and the same results were obtained in the two pretreatment methods.

• 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 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 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.

• Journal of the Korean Society of Tobacco Science
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• v.28 no.1
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• pp.51-57
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• 2006

This study was carried out to improve and evaluate the analytical method for determination of potassium in tobacco leaf by various pre-treatment techniques. The time requirment of various pre-treatments was about 10 hour for dry ashing and 6 hour for microwave digestion and 3 hour for sonication. The results of recover in both pre-treatment techniques, microwave digestion and sonication, is greater than 85 % stably with reproducibility(RSD %) on replicates of less than 3 %. However the mean values for microwave digestion were lower than certified standard value of NlST SRM. Compared to the other pre-treatment techniques, analytical results for sonication technique strictly improved the accuracy and precision. In conclusion, the use of the simple sonication technique seems to be efficient for the determination of potassium in tobacco leaf in consideration for both the accuracy and reproducibility.

• Analytical Science and Technology
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• v.16 no.2
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• pp.152-158
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• 2003

This study was conducted to evaluate two sample digestion procedures and instrumental determination parameters for analysis of lead in bone. Amputated human legs were treated by acid digestion or microwave dissolution prior to spectrometric analysis. Inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GF-AAS) were used for determining bone lead levels. Recovery efficiencies using standard reference material from acid digestion measured by ICP-MS were in good agreement with those of the certified value, but in cases of acid digestion by GF-AAS and microwave digestion by both two methods, recovery underestimated and overestimated, respectively. For the bone samples, the lead concentrations obtained by ICP-MS after acid digestionwere in good agreement with those by GF-AAS (correlation coefficient = 0.983), but GF-AAS gave systematically higher values than ICP-MS. While a good agreement between two analytical methods after microwave digestion was also obtained (correlation coefficient = 0.950), bone lead concentrations from microwave were relatively higher than those from acid digestion. In conclusion, the use of the simple nitric acid digestion procedure at an ambient temperature coupled to ICP-MS seems to be efficient for the determination of lead in bone in consideration for both the convenience and validity.