• Bulletin of the Korean Chemical Society
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• v.24 no.10
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• pp.1433-1436
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• 2003

A new method for the simultaneous determination of heavy metal ions in cigarette material by microwave digestion and reversed-phase high-performance liquid chromatography (RP-HPLC) has been developed. The cigarette material was digested by microwave digestion. Lead, cadmium, mercury, nickel and tin ions in the digested samples were pre-column derivatized with tetra-(2-chlorophenyl)-porphyrin ($T_2$-CPP) to form color chelates, which were then enriched by solid phase extraction with a $C_{18}$ cartridge. The chelates were separated on a Waters Xterra$^{TM}RP_{18}$ column by gradient elution with methanol (containing 0.05 mol/L pyrrolidine-aceticacid buffer salt, pH = 10.0) and acetone (containin0.05 mol/L pyrrolidine-acetic acid buffer salt, pH = 10.0)as mobile phase at a flow rate of 0.5mL/min and analyzed with a photodiode array detector from 350-600 nm. The detection limits of lead, cadmium, mercury, nickel and tin were 4,3,3,8 and 5 ng/L, respectively, in the original samples. This method was afforded good results.

• Journal of the Korean Society of Tobacco Science
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• v.30 no.1
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• pp.25-32
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• 2008

In this study, we compared three different pretreatment methods, such as block digestion, microwave digestion and solvent injection, coupled with Octopole Reaction System(ORS)-ICP-MS was used for the quantification of heavy metals in mainstream smoke of 2R4F reference cigarette, and then evaluated those efficiencies in the recovery, repeatability and reproducibility. In all methods, volatile heavy metals, As, showed the highest CV value, and Cd showed the lowest one. However, the solvent injection method showed the most stable recovery rate and CV value of 2.36 %. This method showed also advantages in time-consuming and compatibility with ICP-MS system. This results demonstrate that solvent injection method can be recommended as a superior pretreatment procedure to be able to reduce contaminants and spectral interference as well as loss of the elements interested.

• Analytical Science and Technology
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• v.14 no.2
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• pp.173-179
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• 2001

The study was carried out to analyze the pollutant Fe, Cu, Cr, Zn, Cd for sediments collected from lake in K river basin. Three analytical methods currently used in Korea, Japan, U.S.A, were compared. Pretreatment using microwave digestion showed higher analytical results for Fe, Cu, Cr, Zn, Cd than Korean Official Method(KOM) and American Toxicity Characteristic Leaching Procedure(TCLP) Method. Also, analytical results using microwave digestion, TCLP and KOM were as follows: 38.1-48.0 mgFe/kg, 10.2-15.9 mgFe/kg AND 3.5-12.6 mgFe/kg, 37.0-50.1 mgCu/kg, 0.06-0.24 mgCu/kg and 0.01-0.03 mgCu/kg, 137.0-152.0 mgZn/kg, 0.67-0.82 mgZn/kg and 0.3-0.5 mgZn/kg, respectively. From this result, a new analytical method for the determination of heavy metal in sediment should be developed for the accurate estimation of pollution degree in sediment.

• 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.

• The Journal of the Petrological Society of Korea
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• v.3 no.1
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• pp.41-48
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• 1994

Three USGS rock standards (G-2, W-2, and BHVO-1) are decomposed by three different methods, such as open beaker, microwave oven, and alkali fusion method, to compare the effect of decomposition methods for trace elememt analysis in the rock samples. Solubilized trace elements are measured with inductively coupled plasma mass spectrometer (ICP-MS). Generally the analytical results of trace elements between open beaker and microwave digestion method are not different. In case of alkali fusion method, some volatile elements such as Pb, Cu, and Rb are considerably lost. Using acid digestion method, Zr and Hf concentrations are lowered in case that these elements are concentrated in refractory minerals. The concentrations of rare earth elements are generally consistent with the recommended values, but due to large dilution factor, there are some analytical problems in alkali fusion method.

• Analytical Science and Technology
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• v.11 no.4
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• pp.281-291
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• 1998

An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in blood and urine has been investigated by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Microwave oven was used for the pretreatment of blood samples using nitric acid and hydrogen peroxide in a closedvessel digestion system with 1 mL whole blood for 8 minutes. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Detection limits for Cu, Sn, and Bi by this method were 0.000375 ng/mL, 0.000297 ng/mL, and 0.000174 ng/mL, respectively. Recoveries of 99.1% for Cu, 102.5% for Sn, and 98.4% for Bi were obtained for the standard spiked NIST SRM 955a blood sample. The developed method was applied for whole real blood and urine samples.

• Journal of Food Hygiene and Safety
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• v.28 no.1
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• pp.45-49
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• 2013

This study aimed to determine heavy metal contents in sesame oil samples produced in Korea through microwave-assisted acid digestion without using an emulsifier. Three heavy metal, cadmium (Cd), lead (Pb) and arsenic (As) in twelve sesame oil samples were determined by ICP-MS. The validation of analysis method was checked by standard addition method (10 and $100{\mu}g/kg$). As a result, linearity ($R^2$) was above 0.999 and RSDs were lower than 4%. The recovery of Cd, Pb and As ranged between 98.5-101.6%, 100.3-101.3%, and 102.1-111.2%, respectively. The detected ranges in sesame oil samples were as follows; N.D. to $0.109{\mu}g/g$ for Cd, 0.014 to $0.200{\mu}g/g$ for Pb and 0.014 to $0.125{\mu}g/g$ for As, respectively. Therefore, sesame seeds and products grown in heavy metal-polluted regions which are used as food should be given priority attention and consideration.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.42 no.5
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• pp.67-73
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• 2010

Paper packaging materials are essential in protection and transportation of commercial or industrial products. Raw materials for packaging paper production are mainly obtained from various grades of waste paper. For this reason, the recycled fibers from waste paper would probably have possibility of containing heavy metals. This study was focused on the development of optimum pre-treatment method for the quantitative analysis of mercury. The optimum pre-treatment for open digestion system were obtained at the treatment conditions of acid combination with $HNO_3/HCl/H_2O_2$ or $HNO_3/H_2SO_4$ at $80^{\circ}C$. The optimum pre-treatment conditions in closed digestion system were determinated by the acid combination with $HNO_3/HCl/H_2O_2/HF$ in microwave at 320 W for 20 min. The recovery rate in open digestion system was 85~94% and in closed digestion system was indicated as about 100%. Therefore, the closed system is superior than the open system in pre-treatment method for the quantitative analysis of mercury, and the detected mercury contents in the sample of KOCC, AOCC and kraft sack paper were measured below 1 ppm.

• Analytical Science and Technology
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• v.36 no.5
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• pp.216-223
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• 2023

Aluminium (Al) is one of the major elements in rocks and its concentration can be varied, depending on different rock types as well as sources. The present study aimed to propose an analytical method based on the UV-Vis as a cheap, simple, and common instrument equipped in most laboratories for Al quantification in rocks after the microwave assisted acid digestion. The aluminone and 8-hydroxyquinoline were investigated for the colorimetric assay. The results show that the 8-hydroxyquinoline reagent was more favorable in terms of the minimized affects of the potential interferences present in the digested solutions, i.e., Fe³⁺, Si⁴⁺ and F^-. The calibration curve was constructed from 0.10 mg/L to 3.00 mg/L with the goodness of linearity (R² = 0.9996). The limits of detection and quantification (LOD and LOQ) were estimated, i.e., 0.029 mg/L and 0.087 mg/L, respectively. The 8-hydroxyquinoline was applied to real rock samples, demonstrating favorable precision (RSD = 0.34 %-1.8 %) and no remarkable differences were found compared to the inductively coupled plasma-mass spectrometry (ICP-MS) as a reference measurement approach.

• Analytical Science and Technology
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• v.10 no.4
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• pp.240-245
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• 1997

An accurate analysis method for the determination of lead in whole blood by ICP/MS was developed. Whole blood samples were decomposed in microwave digestion system without any contamination and loss of lead. The 96 samples were analyzed by ICP/MS using mass$^{208}$ isotope of lead. Lead concentrations of human whole blood were ranged of $2.50{\sim}22.8{\mu}g/dL$. The accuracy of this analysis method was verified by analyzing of NIST SRM 955a series(lead in blood).