• 대한방사선방어학회:학술대회논문집
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• 대한방사선방어학회 2010년도 춘계 학술발표회 및 심포지엄
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• pp.86-87
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• 2010

• Mass Spectrometry Letters
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• 제11권4호
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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.

• 한국원자력학회:학술대회논문집
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• 한국원자력학회 1999년도 춘계학술발표회요약집
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• pp.394-394
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• 1999

• 분석과학
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• 제27권3호
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• pp.140-146
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• 2014

후 컬럼 동위원소 희석법(PCID, post column isotope dilution)을 HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry)에 적용한 정량법에서 내부 표준물을 동시에 사용하여 정확도와 정밀도를 개선하였다. 전통적인 여러 정량법과 후 컬럼 동위원소 희석법을 비교하여 볼 때에 PCID의 경우에 컬럼내에서 발생하는 오차가 가장 큰 요인으로 작용하였음을 알 수 있었다. PCID에서 내부 표준물을 사용하여 컬럼내에서의 손실에 대한 오차를 효과적으로 보정하고 정확도와 정밀도를 개선할 수 있었다. 셀레늄 화학종인 SeMet을 시료로 사용하고 내부 표준물로 MeSecys 또는 $Se^{4+}$를 이용한 결과, 사용하지 않은 경우와 비교하면 상대오차는 각 각 31%와 13%에서 모두 1% 대로 낮아져 정확도가 크게 개선되었으며, 상대 표준편차는 5.1%와 6.9%에서 각각 1.5%와 0.2%로 정밀도 또한 크게 개선되었다. PCID에서 내부 표준물을 사용하였을 때의 정량분석법의 장점을 다른 분석법과 비교 토의하였다.

• 한국환경과학회:학술대회논문집
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• 한국환경과학회 2016년도 정기학술대회 발표논문집
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• pp.134-134
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• 2016

• Bulletin of the Korean Chemical Society
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• 제34권12호
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• pp.3817-3824
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• 2013

Various separation modes in HPLC, such as anion exchange (AE), reversed-phase (RP), and affinity (AF) chromatography were examined for the separation of selenium species in human blood serum and urine. While RP- and AE-HPLC were mainly used for the separation of small molecular selenium species, double column AF-HPLC achieved the separation of selenoproteins in blood serum efficiently. Further, the effluent of AF-HPLC was enzymatically hydrolyzed and then analyzed with RP HPLC for selenoamino acid study. The versatility of the hybrid technique makes the in-depth study of selenium species possible. For quantification, post column isotope dilution (ID) with $^{78}Se$ spike was performed. ORC ICP/MS (octapole reaction cell inductively coupled plasma/mass spectrometry) was used with 4 mL $min^{-1}$ Hydrogen as reaction gas. In urine sample, inorganic selenium and SeCys were identified. In blood serum, selenoproteins GPx, SelP and SeAlb were detected and quantified. The concentration for GPx, SelP and SeAlb was $22.8{\pm}3.4\;ng\;g^{-1}$, $45.2{\pm}1.7\;ng\;g^{-1}$, and $16.1{\pm}2.2\;ng\;g^{-1}$, respectively when $^{80}Se/^{78}Se$ was used. The sum of these selenoproteins ($84.1{\pm}4.4\;ng\;g^{-1}$) agrees well with the total selenium concentration measured with the ID method of $87.0{\pm}3.0\;ng\;g^{-1}$. Enzymatic hydrolysis of each selenium proteins revealed that SeCys is the major amino acid for all three proteins and SeMet is contained in SeAlb only.

• Mass Spectrometry Letters
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• 제3권2호
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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.

• 분석과학
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• 제21권5호
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• pp.364-374
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• 2008

2000년도에 COMNAP/SCAR에 의해 극지지역의 환경모니터링에 관한 표준기술지침서인 'Antarctic Environmental Monitoring Handbook'이 발간되었다. 이 지침서에 따라 남극세종기지주변지역의 토양시료중의 중금속을 분석하였다. 시료분해방법은 고압산분해 방법을 사용하였고, 분석방법으로는 동위원소희석 유도결합플라스마질량분석법을 사용하여 토양중의 Pb, Cu, Zn 성분을 분석하였다. 분석방법의 정확성을 확인하기 위해 표준시료인 NIST 2702를 분석한 결과 인증값의 99.5~100.8% 범위내에서 일치하였다. Chelex 100 이온교환수지를 사용하여 간섭이온을 제거하기 위해 매질을 분리하였다. 측정결과 인위적오염이 예상되는 기지주변지역의 중금속의 평균농도는 각각 Pb 332.9 mg/kg, Cu 95.6 mg/kg, Zn 115.3 mg/kg로 나타났으며, 기지에서 멀리 떨어진 지역의 평균농도는 각각 Pb 28.1 mg/kg, Cu 101.8 mg/kg, Zn 115.6 mg/kg로 나타났다. Pb 농도는 기지주변지역과 멀리 떨어진 지점에서 현저한 차이를 보였다.

• Bulletin of the Korean Chemical Society
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• 제35권12호
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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.

• 분석과학
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• 제13권3호
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• pp.297-303
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• 2000

저니토 시료 중의 미량 Cd, Cu, Pb, Ni, Zn 등의 분석을 위해 동위원소희석 질량분석법을 이용하였다. 시료는 마이크로파 혼합산(질산, 불산, 과염소산) 분해법을 이용하여 용해하였다. Ammonium pyrrolidenedithiocarbamate(APDC) 용매 추출법을 이용하여 알칼리 및 알칼리 토금속을 분리한 다음 Pb를 측정하고, 나머지 원소들은 이 용액에 $NH_4OH$ 첨가 후 원심 분리하여 Fe, Sn, Ti 등을 제거한 다음 측정하였다. 측정원소의 회수율은 다소 떨어지나 동중원소 방해를 일으키는 매질원소를 효율적으로 제거할 수 있었다. 2종의 저니토 인증표준물질 중의 미량원소 분석에 이 방법을 적용한 결과 인증값과 잘 일치하는 측정 결과를 얻을 수 있었다.