• Journal of environmental and Sanitary engineering
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• v.16 no.1
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• pp.91-101
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• 2001

In order to propose a optimum method increasing accuracy and reproducibility in analysis of urine lead levels, we compared matrix modifier addition method and microwave digestion method. The results were as follows ; 1. Where the concentration of $Pd(NO_3)_2$(matrix modifier) was $50mg/{\ell}$, and ashing temperature was $900^{\circ}C$, the results were optimum. In case of matrix modifier addition method, the average coefficient of variation (CV) of normal man was 24.1%, and lead worker was 7.9%. The average urine lead levels of standard were $10.42\mu{g}/{\ell}$ and $19.89\mu{g}/{\ell}$ , the accuracies compared to reference values were 97.0% and 92.6%, respectively. 2. Microwave digestion temperature($160~180^{\circ}C$), time(15~25min) and the ratio of urine/ashing acid(1:1~4:1) did not significantly affect lead absorbance and background absorbance. Therefore we set up a optimum analytical conditions as follows: temperature, $160^{\circ}C$; time, 15min; the ratio of urine/ashing acid, 4:1. after samples were digested by the above analytical conditions, lead absorbance and background absorbance was measured at $450^{\circ}C$ as ashing temperature. The average coefficient of variation (CV) of normal man was 12.4%, and lead worker was 6.2%. The average urine lead levels of standard urine were $10.66\mu{g}/{\ell}$ and $23.31\mu{g}/{\ell}$, the accuracies compared to reference values were 99.3% and 103.9%, respectively. From the results, we suggest that microwave digestion method is a more favorable method than matrix modifier addition method because of easiness to reduce organic matter, possibility to analysis at low temperature and accuracy.

• Korean Journal of Veterinary Research
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• v.52 no.2
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• pp.69-74
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• 2012

The analytical method of trace toxic metals in livestock products was confirmed and validated through certified reference material (CRM) and the international proficiency tests. There are some difficulties to determine low levels of toxic metals in livestock products because of interferences due to the matrix. The recoveries of CRM (NIST 1577c) ranged from 73.9 to 119% for lead and from 86.4 to 111% for cadmium in bovine liver. The international proficiency tests were carried out with the milk powder and cocoa powder samples including metals provided by Food Analysis Performance Assessment Scheme (FAPAS$^{(R)}$, UK). The test samples were prepared by microwave digestion using solution of $HNO_3:H_2O_2:H_2O$ (v/v/v = 5 : 2 : 4) and analyzed by ICP/MS. The analytical result of cadmium in milk powder was $121{\mu}g/kg$ with -0.3 of the z-score compared to the assigned value of $131{\mu}g/kg$ by FAPAS$^{(R)}$. The analytical results of lead and cadmium in cocoa powder were $29.2{\mu}g/kg$ and $97.6{\mu}g/kg$, respectively, which satisfied the assigned values of $34.2{\mu}g/kg$ for lead and $126{\mu}g/kg$ for cadmium by FAPAS$^{(R)}$. It is verified that the analytical method is accurate and reliable to determine trace lead and cadmium in livestock products by microwave digestion and ICP/MS.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.26 no.1
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• pp.48-57
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• 2016

Objectives: This study was conducted to evaluate the accuracy and precision of airborne metal analysis using polyvinyl chloride(PVC) membrane filter by pretreatment methods. Methods: A total of 75 spiked PVC samples for Cr, Fe and Mn ranged from 6 ug/sample to 40 ug/sample were used to evaluate recovery rates for three pretreatment methods: acid extraction, hot plate ashing and microwave digestion. For Mn, an additional 75 spiked mixed cellulose ester(MCE) membrane filters were analysed to compare the recovery rates of PVC samples. All samples were analysed with an inductively coupled plasma optical emission spectrometer(ICP-OES) and manganese samples were additionally analyzed by atomic absorption spectrometer(AAS). Results: The overall mean recovery rates of PVC samples for Cr, Fe and Mn were 90% or higher regardless of pretreatment methods, but there were statistically significant differences in recovery rates for Cr(p<0.05) and Mn(p<0.01) samples by pretreatment methods. The biases and the coefficient variations of PVC samples for three metals pretreated with three kinds of pretreatment methods ranged from 1.7% to 4.7% and from 1.6% to 6.5%, respectively. The manganese PVC samples pretreated by microwave digestion and analyzed with ICP-OES had the lowest bias at 1.9% and also showed lower bias than the bias for MCE samples, 2.7%. Conclusions: In order to accurately analyze the metals sampled with PVC membrane filters, microwave digestion and ICP-OES can be recommended.

• Journal of The Korean Society of Agricultural Engineers
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• v.62 no.2
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• pp.17-29
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• 2020

The objective of this study was to find an optimum methane yield condition in anaerobic digestion of sewage sludge with microwave pretreatment. The pretreatment process was carried out using a lab scale industrial microwave unit (2,450 MHz frequency). The digestion efficiency of pretreated sludge was evaluated by biochemical methane potential (BMP) test. Box-Behnken design and Response Surface Analysis (RSA) were applied to determine the optimal combination of sludge mixing ratio (0 to 100%), power (400 to 1600 W), holding time (0 to 10 min) and pretreatment temperature (60 to 100℃). BMP test results showed that Volatile Solid (VS) removal efficiency was up to 48% at a condition of 0% for mixing ratio, 1600 W for power, 5 min for holding time, and 80℃ for pretreatment temperature. Methane production was up to 832.3 mL/g VS_removed at a condition of 50% for mixing ratio, 1000 W for power, 5 min for holding time, and 80℃ for pretreatment temperature. The results of the variance analysis (ANOVA) showed that the p-value of the power and pretreatment temperature among the independent variables were significant (p<0.05), and in particular, the pretreatment temperature significantly affected on the solubilization and methane production. The optimum condition for the maximum methane yield (847 mL/g VS_removed) was consist of 38.4% of mixing ratio, 909.1 W of power, 4.1 min of holding time, and 80℃ of temperature within the design boundaries.

• 한국생물공학회:학술대회논문집
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• 2003.04a
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• pp.128-131
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• 2003

The effect of microwave irradiation on waste activated sludge was investigated in order to improve solubilization. a different levels of microwave irradiation time were varied within a range from 1 min to 15 min. When WAS was pretreated at 1, 3, 5, 7, and 15 min, the SCOD concentration increased according to microwave irradiation time. A simple batch procedure was used to measure the VFA potential, i.e. the amount of VFA that can be formed through digestion of organic constituent in sludge. At equilibrium point, TVFA in the case of 1, 3, 5, 7 and 15 min microwaved sludges was 8%, 122%, 243%, 279% and 232% higher than that in the case of raw sludge, respectively.

• Analytical Science and Technology
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• v.25 no.6
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• pp.402-409
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• 2012

Quantitative analytical condition for arsenic in plastic materials by the flow injection-hydride generation-inductively coupled plasma-atomic emission spectrometry was studied. The plastic samples were dissolved by wet-acid digestion method and microwave-acid digestion method. The reproducibility and accuracy in this method was verified using of certified reference materials(CRMs) CRM-EC680k and CRM-EC681k. The analyical results agrees with certified value within the range of uncertainty. The results of CRM-EC680k wer 4.1~4.3 mg/kg (certified value $4.1{\pm}0.5$ mg/kg), and the results of CRM-EC681k were 28.9~30.6 mg/kg (certified value $29.1{\pm}1.8$ mg/kg).

• Journal of Korean Society for Atmospheric Environment
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• v.21 no.4
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• pp.423-430
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• 2005

This study was investigated with sample digestion techniques and a reliability of the analytical results for a quantitative analysis of a standard reference material ('urban particulate matter', SRM 1648). The metallic elements were analyzed by inductively coupled plasma mass spectrometry (ICP-MS) with closed vessel microwave acid digestion method and atomic absorption spectroscopy (AAS). Quality control of the overall analytical procedures for metallic element determinations of standard reference material were estimated by analysis of a SRM 1648. Three digestion solutions $(type\;1:\;HNO_3,\;type\;2:\;HNO_3\;and\;H2O_2(4'1)\;mixture,\;type\;3:5.55\%\; HNO_3\;and\;16.75\%\;HCI\;mixture)$ were applied to SRM 1648. As a result, three digestion solutions used in this study are completely unable to digest Cr of SRM 1648. Reliability of Cr and As showed some errors in the digestion with digestion solution type (3) due to the influence of chlorides. Type (3) digestion solutions are sufficient to fulfill the digestion of As as well as Se in SRM 1648. ICP-MS results showed the improvement in accurate and precise determination of some trace elements like Cd, V and Pb in SRM 1648. It is important to use the proper digestion solution for each element to qualify analytical precision.

• Analytical Science and Technology
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• v.11 no.4
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• pp.297-304
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• 1998

The three analysis methods, EPA method 3050, the method offered by Ministry of Environment in Korea, and modified method corrected in this laboratory, were studied to investigate the effect of matrix on the analysis of inorganic priority pollutants. 7 inorganic priority pollutants(Ni, Cr, Cu, Zn, Pb, Cd, Hg) were spiked to the plating, leather, paper, electric, and dye sludges. Mean recovery of the elements except Hg was 95.5% when the procedure of EPA method was applied. However, recovery by the two other extraction methods showed 11.1% and 27.7%, respectively. Digestions were done by MDS (microwave digestion system) and $HNO_3+HClO_4$ methods. To study organic and inorganic matrix effect, samples were made by adding triethanol amine as a organic matrix and $FeCl_3{\cdot}6H_2O$+$AlCl_3{\cdot}6H_2O$ as a inorganic matrix, respectively. The extracts were analyzed by AAS and HG-AAS. Mean recovery of the elements by the $HNO_3+HClO_4$ procedure, except Hg, gave better result than that of the MDS method. Mean recovery of elements was decreased when organic and inorganic matrices were added in the sludge samples. The procedure of MDS and $HNO_3+HClO_4$ digestion gave higher recoveries than that of direct analysis. In general, the results of the studies showed a significant matrix effect on the inorganic priority pollutants analysis in sludges.

• Proceedings of the Korean Radioactive Waste Society Conference
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• 2019.05a
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• pp.401-402
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• 2019

• Proceedings of the Korean Radioactive Waste Society Conference
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• 2017.05a
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• pp.281-282
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• 2017