• Journal of Korean Society for Atmospheric Environment
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• v.9 no.3
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• pp.247-254
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• 1993

A simple and direct method is developed for the determination of light Elements in atmospheric particulates by X-ray fluorescence spectrometry. Calibration standards for the light elements such as Al, Mg, K, Ca, etc are prepared by filtering real atmospheric particulates over variable time and subsequently standardizing them by Inductively Coupled Plasma-Mass Spectrometry(ICP-MS) or Atomic Absorption Spectrophotometry(AAS) analysis. The validity of this calibration method is tested by analyzing more than 100 aerosol samples, collected at urban(Seoul) and rural(Padori) sites over a two year period with this method and then comparing them with those by other accuracy proven methods such as AAS or ICP-MS: for all metals tested the results showed reasonably good agreements (R $\geq$ 0.95).

• Mass Spectrometry Letters
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• v.11 no.4
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• pp.108-112
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• 2020

A certified reference material (CRM) for the analysis of nutrient elements in an edible mushroom (Ganoderma lyceum) powder has been developed (KRISS CRM 108-10-011). The mass fractions of calcium (Ca), iron (Fe), and zinc (Zn) were measured by isotope dilution inductively coupled plasma mass spectrometry (ID ICP/MS). To dissolve the fungi cell wall of mushroom consisted of chitin fibers, sample preparation method by single reaction chamber type microwave-assisted acid digestion with acid mixtures was optimized. The mean measurement results obtained from 12 sample bottles were used to assign as the certified values for the CRM and the between-bottle homogeneities were evaluated from the relative standard deviations. The certified values were metrologically traceable to the definition of the kilogram in the International System of Units (SI). This CRM is expected to be used for validation of analytical methods or quality control of measurement results in analytical laboratories when they determine the mass fractions of elements in mushroom or other similar samples.

• Bulletin of the Korean Chemical Society
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• v.22 no.2
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• pp.205-209
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• 2001

Uniformly-doped silicon thin films were fabricated by ion beam sputter deposition. The thin films had four levels of copper dopant concentration ranging between 1 ${\times}$1019 and 1 ${\times}$ 1021 atoms/cm3 . Concentrations of Copper dopants were determined by the isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) to provide certified reference data for the quantitative surface analysis by secondary ion mass spectrometry (SIMS). The copper-doped thin films were dissolved in a mixture of 1 M HF and 3 M HNO3 spiked with appropriate amounts of 65 Cu. For an accurate isotope ratio determination, both the detector dead time and the mass discrimination were appropriately corrected and isobaric interference from SiAr molecular ions was avoided by a careful sample pretreatment. An analyte recovery efficiency was obtained for the Cu spiked samples to evaluate accuracy of the method. Uncertainty of the determined copper concentrations, estimated following the EURACHEM Guide, was less than 4%, and detection limit of this method was 5.58 ${\times}$ 1016 atoms/cm3.

• Analytical Science and Technology
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• v.27 no.3
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• pp.140-146
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• 2014

An internal standard was used in PCID (post column isotope dilution) to improve the accuracy and precision in quantification of various chemical species. The error occurring in the column was the largest in HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry) when PCID and other traditional quantification methods were compared with each other. Internal standard was effective in correcting the loss of sample in the column to improve accuracy and precision. When applied to SeMet, using MeSecys or $Se^{4+}$ as an internal standard, relative errors were reduced from 31% and 13% to less than 1%, while standard deviations were reduced from 5.1% and 6.9% to 1.5% and 0.2%, respectively. Positive aspects of using an internal standard in PCID were compared with other quantitative techniques and discussed in detail.

• Nuclear Engineering and Technology
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• v.45 no.3
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• pp.415-420
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• 2013

A determination method for $^{237}Np$ in spent nuclear fuel samples was developed using an isotope dilution method with $^{239}Np$ as a spike. In this method, inductively coupled plasma mass spectrometry (ICP-MS) was taken for the $^{237}Np$ instead of the previously used alpha spectrometry. $^{237}Np$ and $^{239}Np$ were measured by ICP-MS and gamma spectrometry, respectively. The recovery yield of $^{237}Np$ in synthetic samples was $95.9{\pm}9.7$% (1S, n=4). The $^{237}Np$ contents in the spent fuel samples were 0.15, 0.25, and $1.06{\mu}g/mgU$ and these values were compared with those from ORIGEN-2 code. A fairly good agreement between the measurements (m) and calculations (c) was obtained, giving ratios (m/c) of 0.93, 1.12 and 1.25 for the three PWR spent fuel samples with burnups of 16.7, 19.0, and 55.9 GWd/MtU, respectively.

• Mass Spectrometry Letters
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• v.3 no.2
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• pp.58-61
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• 2012

A method based on flow injection-isotope dilution-cold vapor-inductively coupled plasma mass spectrometry (FI-IDCV-ICP/MS) has been applied to determine trace level of mercury in fly ash. $^{200}Hg$ isotopic spike was added to 0.25 g of BCR176R fly ash and then decomposed by microwave digestion procedure with acid mixture A (8 mL $HNO_3$ + 2 mL HCl + 2 mL HF) and acid mixture B (8 mL $HNO_3$ + 2 mL $HClO_4$ + 2 mL HF) for applying IDMS. Mercury cold vapor was generated by using reductant solution of 0.2% (w/w) $NaBH_4$ and 0.05% (w/w) NaOH. The measurements of n($^{200}Hg$)/n($^{202}Hg$) isotope ratio was made using a quadrupole ICP/MS system. The accuracy in this method was verified by the analysis of certified reference material (CRM) of fly ash (BCR 176R). The indicative value of Hg in BCR 176R fly ash was $1.60{\pm}0.23$ mg/kg (k = 2). The determined values of Hg in BCR 176R fly ash by the method of FI-CV-ID-ICP/MS described in this paper were $1.60{\pm}0.24$ mg/kg (k = 3.18) and the analysis results were in well agreement with the indicative value within the range of uncertainty.

• Analytical Science and Technology
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• v.15 no.4
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• pp.335-340
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• 2002

An analytical method has been developed to determine multi-elements in human hair samples by inductively coupled plasma mass spectrometry (ICP-MS). 0.05 g of hair sample was added to the Teflon digestion bomb together with 1.5 mL of nitric acid and an appropriate amount of In as an internal standard. The sample was then decomposed in the microwave digestion system. The hair certified reference material, GBW 09101, was analyzed for the validation of the analytical method. The determined values were in good agreement with the certified values within the uncertainty range.

• Mass Spectrometry Letters
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• v.4 no.4
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• pp.87-90
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• 2013

Isotope amount ratios of lead in a bronze sample have been successfully determined using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS). Matrix separation conditions were tested and optimized using ion exchange chromatography with anion-exchange resin, AG1-X8, and sequential elution of the 0.5 M HBr and 7 M $HNO_3$ to separate lead from very high contents of copper and tin in bronze matrix. Mercury was also removed efficiently in the optimized separation condition. The instrumental isotope fractionation of lead in the MC-ICP-MS measurement was corrected by the external standard sample bracketing method using an external standard, NIST SRM 981 lead common isotope ratio standard followed by correction of procedure blank to obtain reliable isotope ratios of lead. The isotope ratios, $^{206}Pb/^{204}Pb$, $^{207}Pb/^{204}Pb$, $^{208}Pb/^{204}Pb$, and $^{208}Pb/^{206}Pb$, of lead were determined as $18.0802{\pm}0.0114$, $15.5799{\pm}0.0099$, $38.0853{\pm}0.0241$, and $2.1065{\pm}0.0004$, respectively, and the determined isotope ratios showed good agreement with the reference values of an international comparison for the same sample within the stated uncertainties

• Proceedings of the KSEEG Conference
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• 2001.04a
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• pp.349-349
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• 2001

• Bulletin of the Korean Chemical Society
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• v.23 no.11
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• pp.1541-1544
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• 2002

The concentration of B in steels is important due to its influence on mechanical properties of steel such as hardenability, hot workability, and creep resistance. An analytical method has been developed to determine B in steel samples by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). National Institute of Standard and Technology Standard Reference Material (NIST SRM) 348a was analyzed to validate the analytical method. The steel sample was digested in a centrifuge bottle with addition of aqua regia and $^{10}B$ spike isotope. Sample pH was then adjusted to higher than 10 to precipitate most matrix elements such as Fe, Cr, and Ni. After centrifugation, the supernatant solution was passed through a cation exchange column to enhance the matrix separation efficiency. B recovery efficiency was about 37%, while matrix removal efficiency was higher than 99.9% for major matrix elements. The isotope dilution method was used for quantification and the determined B concentration was in good agreement with the certified value.