• Journal of Environmental Health Sciences
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• v.47 no.1
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• pp.64-77
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• 2021

Objective: Biological monitoring of trace elements in human blood samples has become an important indicator of the health environment. The purpose of this study was to detect and evaluate multiple metal items in blood samples based on ICP-MS, to perform comparative evaluation with the existing analysis method, and to develop and verify a new method. Methods: 100 μL of whole blood from 80 healthy subjects was used to analyze ten metals (Sb, tAs, Cd, Pb, Mn, Hg, Mo, Ni, Se, Tl) using ICP-MS. Verification of the analysis method included calculation of linearity, accuracy, precision and detection limits. In addition, a comparative test with the conventional graphite furnace atomic absorption spectroscopy (GF-AAS) method was performed. In the case of Pb, Cd, and Hg in whole blood, cross-analysis between Pb, Cd, and Hg analysis methods was performed to confirm the difference between the existing method and the new method (ICP-MS). Results: The coefficient of determination (R2) was 0.999 or higher in seven items and 0.995 or higher in three items. The Pb result showed that Pearson's correlation coefficient was very high at 0.983, and the intraclass correlation coefficient was 0.966. The Cd result showed that Pearson's correlation coefficient was 0.917 between the existing method and the new analysis concentration value. Its intraclass correlation coefficient was 0.960, and there was no significant difference between the two groups. Hg had a low correlation at 0.687, and the intraclass correlation coefficient was 0.761, which was lower than that of Pb and Cd. The intra-day and inter-day accuracy of Pd and Cd were satisfactory, but Hg did not meet the criteria for both accuracy and precision when compared with the conventional analysis method. Conclusion: This study can be meaningful in that it proposes a more efficient and feasible analysis method by verifying a blood heavy metal concentration experiment using multiple simultaneous analyses. All samples were processed and analyzed using the new ICP-MS. It was confirmed that the agreement between the two methods was very high, with the agreement between the current and new methods being 0.769 to 0.998. This study proposes an efficient simultaneous methodology capable of analyzing multiple elements with small samples. In the future, studies of various applications and the reliability of ICP-MS analysis methods are required, and research on the verification of accurate, precise, and continuous analysis methods is required.

• Proceedings of the Korea Air Pollution Research Association Conference
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• 2002.11a
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• pp.239-240
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• 2002

유해 대기오염물질에 대한 수용 모델링을 위해 대규모의 분진시료에 대한 분석이 필수적이나 현재로서는 미미한 실정이다. 대규모의 분진시료를 대상으로 미량금속을 분석하기 위해 기존 국내 연구에서 사용된 XRF, ICP-AES, PLXE 분석법 대신 검출 한계가 매우 낮고 재현성이 뛰어난 중성자 방사화 분석법(INAA)과 플라스마 분광법(ICP-MS)을 이용하여 대기오염분야에의 적용성을 평가하는 것은 매우 유용한 연구일 것으로 판단된다. (중략)

• Bulletin of the Korean Chemical Society
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• v.16 no.5
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• pp.422-427
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• 1995

In a stream of water sample, trace metal ions are quantitatively coprecipitated with Indium hydroxide and filtered. The filtered precipitate is continuously dissolved in 3 M nitric acid and introduced to ICP directly. The lead, cadmium, and copper are concentrated more than 10-fold and determined with ICP-AES at a sampling frequency of 10/hour. The detection limits are 2.89, 1.43,0.52 ppb for lead, cadmium, and copper respectively. Recoveries of lead, cadmium, and copper are 98.7, 94.3, and 104.5% respectively. The RSD values for three elements are about 3-5% currently.

• Analytical Science and Technology
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• v.14 no.4
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• pp.311-316
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• 2001

We have investigated the trace amount in an oriental medicine in oder to determine the geographical origin by using inductively coupled plasma-atomic emission spectrometry(ICP-AES) and chemometric anlysis with principal component analysis(PCA) and pattern recognition. Astragali Radix from several agricultural places in Korea was selected as an example of the oriental medicine and analyzed by ICP-AES. The dried Astragali Radix sample was treated with $HNO_3$ and $H_2O_2$, then digested using microwave oven. Elements such as Mg, Al, K, Ca, Ti, Mn, Fe, Cu, Zn, and Ba with different concentrations were found an used for the identification of the origin of agriculture places. Especially, the concentration of Al, Fe, Zn and Ti were employed to investigate the relationship between. Astragali Radix and the agricultural places by PCA and pattern recognition. We have made a program that is based on chemometrics in analytical spectroscopy. The results of the chemometrics analysis indicated that a distinction among Yechon and Chechon, Chungson, Kurye and Chinese Astragali Radix could be made. We believe that principal component analysis(PCA) and pattern recognition is a valuable tool to identify the origin of Astragali Radix in terms of the agricultural place.

• Bulletin of the Korean Chemical Society
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• v.26 no.3
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• pp.440-446
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• 2005

A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

• Analytical Science and Technology
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• v.32 no.4
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• pp.121-130
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• 2019

Alumina is one of the most important ceramic materials because of its useful physical and chemical properties. Recently, high-purity alumina has been used in various industrial fields. This leads to increasing demand for reliable elemental analysis of impurities in alumina samples. However, the chemical inertness of alumina makes the sample preparation for conventional elemental analysis a tremendously difficult task. Herein, we demonstrated the feasibility of laser ablation for effective sampling of alumina powder. Laser ablation performs sampling rapidly without any chemical reagents and also allows simultaneous optical emission spectroscopy and mass spectrometry analyses. For six alumina samples including certified reference materials and commercial products, laser-induced breakdown spectroscopy (LIBS) and laser-ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) analyses were performed simultaneously based on a common laser ablation sampling. LIBS was found to be useful to quantify alkali and alkaline earth metals with limits-of-detection (LODs) around 1 ppm. LA-ICP-MS could quantify transition metals such as Ti, Cu, Zn, and Zr with LODs in the range from a few tens to hundreds ppb.

• Nuclear Engineering and Technology
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• v.50 no.8
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• pp.1349-1354
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• 2018

Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) is widely used for the determination of trace elements in geological samples in Iran. In this paper, we have calculated the detection limits of neutron activation analysis (NAA) for some of the common elements in such samples utilizing the ORIGEN and MCNP codes and verified the simulations using the experimental results of three soil standard reference materials, namely, G02.SRM, G18.SRM, and G28.SRM. The results show that while the detection limit of ICP-AES method is usually in the mg/kg range, it is represented to the ${\mu}g/kg$ range for most of the elements of interest using the NAA method, and the simulations can be verified in a tolerance range of 20%.

• Bulletin of the Korean Chemical Society
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• v.22 no.2
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• pp.159-163
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• 2001

Si3N4 powder has been analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sample was dissolved by high-pressure acid digestion with HF, H2SO4 (1+1), and HNO3 mix ture. This technique is well suited for the impurity analysis of Si3N4 because the matrix interference is eliminated. A round-robin samples trace elements, such as Ca, W, Co, Al, Fe, Mg, and Na, were determined. For the direct analysis, slurry nebulization of 0.96 mm Si3N4 powder also has been studied by ICP-AES. Emission intensities of Fe were measured as ICP operational conditions were changed. Significant signal difference between slurry particles and aqueous solution was observed in the present experiment. Analytical results of slurry injection and high-pressure acid digestion were compared. For the use of aqueous standard solution for calibration, k-factor was determined to be 1.71 for further application.

• The Journal of the Petrological Society of Korea
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• v.24 no.2
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• pp.141-147
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• 2015

Using laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), we evaluated the reliability of trace element abundance data measured from the silicate rock references of JR-3, JG-3, JGb-1 and JB-1b using glass discs made by alkali fusion. For 28 elements including rare earth elements, relative standard deviations (RSD) are better than 7% in case when the concentrations of the elements in the rock samples are greater than 10 ppm. However, RSD shows somewhat increased values for the concentrations less than 10 ppm, but never exceeds 25%. Compared with previously reported averages of the compiled abundance data, our data display satisfactory results for the most cases with differences less than 10%. We suggest that LA-ICP-MS analysis using fused glass beads is a reliable, precise and time-saving method of trace element analysis for the silicate rocks spanning from mafic to felsic compositions.

• Mass Spectrometry Letters
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• v.2 no.4
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• pp.80-83
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• 2011

Isotope ratio analysis of nuclear materials in individual particles is of great importance for nuclear safeguards. Although secondary ion mass spectrometry (SIMS) and thermal ionization mass spectrometry (TIMS) are utilized for the analysis of individual uranium particles, few studies were conducted for the analysis of individual uranium-plutonium mixed oxide particles. In this study, we applied SIMS and inductively coupled plasma mass spectrometry (ICP-MS) to the isotope ratio analysis of individual U-Pu mixed oxide particles. In the analysis of individual U-Pu particles prepared from mixed solution of uranium and plutonium standard reference materials, accurate $^{235}U/^{238}U$, $^{240}Pu/^{239}Pu$ and $^{242}Pu/^{239}Pu$ isotope ratios were obtained with both methods. However, accurate analysis of $^{241}Pu/^{239}Pu$ isotope ratio was impossible, due to the interference of the $^{241}Am$ peak to the $^{241}Pu$ peak. In addition, it was indicated that the interference of the $^{238}UH$ peak to the $^{239}Pu$ peak has a possibility to prevent accurate analysis of plutonium isotope ratios. These problems would be avoided by a combination of ICP-MS and chemical separation of uranium, plutonium and americium in individual U-Pu particles.