• Bulletin of the Korean Chemical Society
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• v.35 no.12
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• pp.3482-3488
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• 2014

Matrix-induced mass bias and its effect on the accuracy of isotope ratio measurements have been examined for a quadrupole-based inductively coupled plasma-mass spectrometer (Q ICP-MS). Matrix-induced mass bias effect was directly proportional to % mass difference, and its magnitude varied for element and nebulizer flow rate. For a given element and conditions in a day, the effect was consistent. The isotope ratio of Cd106/Cd114 under $200{\mu}g\;g^{-1}$ U matrix deviated from the natural value significantly by 3.5%. When Cd 111 and Cd114 were used for the quantification of Cd with isotope dilution (ID) method, the average of differences between the calculated and measured concentrations was -0.034% for samples without matrix ($0.076{\mu}g\;g^{-1}$ to $0.21{\mu}g\;g^{-1}$ for the period of 6 months). However, the error was as large as 1.5% for samples with $200{\mu}g\;g^{-1}$ U. The error in ID caused by matrix could be larger when larger mass difference isotopes are used.

• Journal of Korean Vacuum Science & Technology
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• v.2 no.1
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• pp.49-54
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• 1998

The effect of deposition paratmeters on the solid-phase crystallization of amorphous silicon films deposited by plasma-enhanced chemical vapor deposition has been investigated by x-ray diffraction. The amorphous silicon films were prepared on Si(100) wafers using SiH4 gas with and without H2 dilution at the substrate temperatures between 12$^{\circ}C$ and 38$0^{\circ}C$. The R. F. powers and the deposition pressures were also varied. After crystallizing at $600^{\circ}C$ for 24h, the films exhibited (111), (220), and (311) x-ray diffraction peaks. The (111) peak intensity increased as the substrate temperature decreased, and the H dilution suppressed the crystallization. Increasing R.F. powers within the limits of etching level and increasing deposition pressures also have enhanced the peak intensity. The peak intensity was closely related to the deposition rate, which may be an indirect indicator of structural disorder in amorphous silicon films. Our results are consistent with the fact that an increase of the structural disorder I amorphous silicon films enhances the grain size in the crystallized films.

• 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.16 no.1
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• pp.82-89
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• 2003

Isotope dilution mass spectrometry (IDMS) was applied to the determination of Ni, Cr, Mo in low alloy steel reference materials. The Mo isotope ratio measurement was performed by dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP/MS) using ammonia as a reaction cell gas. In the case of Ni and Cr measurement, all data were obtained at medium resolution mode (m/${\Delta}m=3000$) of double focusing sector field high resolution inductively coupled plasma mass spectrometry (HR-ICP/MS). For the method validation of the technique was assessed using the certified reference materials such as NIST SRM 361, NIST SRM 362, NIST SRM 363, NIST SRM 364, NIST SRM 36b. This method was applied to the determination of Ni, Cr and Mo in low alloy steel sample (CCQM-P25) provided by NMIJ for international comparison study.

• 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.

• 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.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.

• Proceedings of the Materials Research Society of Korea Conference
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• 2002.05a
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• pp.132-132
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• 2002

Diamond is well known as the hardest material in nature. It also has other unique bulk physical and mechanical properties, such as very high thermal conductivity and broad optical transparency, which enable a number of new applications now that large areas of diamond can be fabricated by the new diamond plasma chemical vapor deposition (CVD) technologies. A study on the effects of growth kinetics and properties of diamond films obtained by addition of argon (~7 vol. %) into the methane/hydrogen mixture is carried out using HFCVD system. A negative bias was used as a nucleation enhancement method in addition to the argon dilution. The scanning electron microscopy (SEM) image of surface morphology shows well faceted crystallites with a predominance of angular shapes corresponding to <100> and <110> crystalline surfaces. The nucleation density and growth rate with argon dilution is two orders of magnitude higher than without argon deposition. The Raman spectra show a good quality film whereas XPS spectra show existence of only diamond phase.

• Korean Journal of Materials Research
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• v.7 no.3
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• pp.203-212
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• 1997

This paper evaluated the feasibility of laser consolidation for improving the properties of the plasma coated layer, Further, the mechanim of the degradation sequence of the chrome carbide layer applied on the turbine blades was postualted. The laser consolidation could be successfully applied for improcing the surface properties of the plasma coated blade, if a proper condition was carefully chosen. The consolidated layer had erosion & corrosion resistance and vond strength superiro to those of the as-plasma coated layer. The properties of the consolidated layer were strongly dependent upon the degree of dilution, especially on the Fe pickup from the substrate. The degradation of the plasma coating layer was thought to be a reault of the repeating action of the solid particle erosion, corrosion penetration through the pores and oxide films formed along the interlayer surface and impact spalling.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.21 no.9
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• pp.848-852
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• 2008

Characteristics of microcrystalline-silicon thin-films deposited by plasma-enhanced chemical-vapor deposition (PECVD) method were studied. There were optimum values of RF power density and $H_2$ dilution ratio $(H_2/(SiH_4+H_2))$; maximum grain size of about 35 nm was obtained at substrate temperature of 250 $^{\circ}C$ with RF power density of 1.1 W/$cm^2$ and $H_2$ dilution ratio of 0.91. Larger grain was obtained with higher substrate temperature up to 350 $^{\circ}C$. Grain size dependence on RF power density and $H_2$ dilution ratio could be explained by etching effects of hydrogen ions and changes of species of reactive precursors on growing surface. Surface-mobility activation of reactive precursors by temperature could be a reason of grain-size dependence on the substrate temperature. Microcrystalline-silicon thin-films that could be used for flat-panel electronics such as active-matrix organic-light-emitting-diodes are expected to be fabricated successfully using these results.