• 분석과학
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• 제23권4호
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• pp.389-394
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• 2010

유도결합플라즈마 원자방출분광법 (ICP-AES)을 이용한 모려 (Ostrea gigas) 칼슘의 함량 및 용출 시험 방법을 개발하고 검증하였다. 개발된 분석방법을 사용하여 모려의 총 칼슘 함량을 측정하고, 탄산칼슘 다형 및 칼슘염 조성의 차이에 의해 발생할 수 있는 모려 칼슘의 용출 특성을 평가하였다. 모려 칼슘의 총 함량 범위는 31.8~39.9%이었고, 용출률 변화는 62.7~83.6%이었다 (n=15). ICP-AES 법을 이용한 칼슘 함량 측정을 통해 모려의 품질관리에 적용할 수 있음을 증명하였다.

• KSBB Journal
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• 제25권5호
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• pp.459-465
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• 2010

A simple and efficient analytical method for the simultaneous determination of seven tar color additives was developed using ion pair high performance liquid chromatography. The conditions for HPLC analysis were as follows: column, ${\mu}$-Bondapak C18 (10 ${\mu}m$, 300 ${\times}$ 3.9 mm i.d.); gradient mobile phase, 0.025 mol/L ammonium acetate (containing 0.01 mol/L tetrabutylammonium bromide)-acetonitrile-methanol (65:25:10) as a mobile for fraction A and 0.025 mol/L ammonium acetate (containing 0.01 mol/L tetrabutylammonium bromide)-acetonitrilemethanol (40:50:10) as a mobile for fraction B; flow rate, 1.0 mL/ min; detection wavelength, 254/520/620 nm. We could attain to the detection limits as 0.01~0.05 ${\mu}$g/mL (254 nm) and 0.005~0.01 ${\mu}$g/mL (520 nm) for six red tar color additives, and 0.05 ${\mu}$g/mL (254 nm) and 0.002 ${\mu}$g/mL (620 nm) for Fast green FCF. This analytical method was applicable to determine the tar color additives contained in several commercial cold syrups.

• 분석과학
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• 제16권1호
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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.

• 분석과학
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• 제13권1호
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• pp.22-26
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• 2000

2-Hydroxybenzaldehyde-5-nitro-pyridylhydrazone (2HB-5NPH)를 합성하여 계면활성제 하에서 바나듐 이온(IV)의 분광학적 정량에 응용하였다. pH, 용매효과, 리간드 농도와 계면활성제의 최적조건을 구하였다. 이 과정을 혼합 시료와 실제 시료 중의 바나듐(IV) 정량에 적용하여 만족한 결과를 얻었다(회수율 ${\geq}$ 97% ; $0{\sim}1.5{\mu}g/mL$ 농도 범위에서 상대 표준 편차 ${\leq}$ 3.0% ; 용액중에서 검출 한계 $0.02{\mu}g/mL$).

• Safety and Health at Work
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• 제12권2호
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• pp.209-216
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• 2021

Background: The article presents the results of studies performed in order to develop a new method of airborne potassium bromate(V) determination at workplaces. Methods: The method is based on a collection of the inhalable fraction of potassium bromate(V) using the IOM Sampler, then extraction of bromates with deionized water and chromatographic analysis of the obtained solution. The analysis was performed using ion chromatography with conductometric detection. The tests were performed on a Dionex IonPac®AS22 analytic column (250 × 4 mm, 6 ㎛) with AG22 precolumn (50 × 4 mm 11 ㎛). Results: The method provides for potassium bromate(V) determination within the concentration range of 0.043 ÷ 0.88 mg/m³ for an air sample of 0.72 m³ in volume, i.e., 0.1-2 times the exposure limit value as proposed in Poland. The method was validated in accordance with PN-EN 482. The obtained validation data are as follows: measuring range: 3.1-63.4 ㎍/mL, limit of detection (LOD) = 0.018 ㎍/mL and limit of quantification (LOQ) = 0.053 ㎍/mL. The developed method has been tested in the work environment, on laboratory employees having contact with potassium bromate(V). Conclusion: The analytical method allowed the determination of the inhalable fraction of airborne potassium bromate(V) at workplaces and can be used to assess occupational exposure.

• 분석과학
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• 제20권1호
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• pp.55-60
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• 2007

A sensitive technique for the determination of trace Cu(II) in various samples after the column preconcentration by adsorbing its N-benzoylphenylhydroxylamine (BPHA) onto benzophenone was developed. Several experimental conditions such as the pH of the sample solution, the amount of chelating agent, the amount of benzophenone, and the flowrate of sample solution and so forth were optimized. The interfering effects of diverse concomitant ions were investigated. Fe(III) and $CN^-$ interfered with more seriously than any other ions. However, the interference by these ions could be overcome sufficiently by adjusting the added volume of 0.01M BPHA to 10 mL. The dynamic range, the correlation coefficient ($r^2$) and the detection limit obtained by this proposed technique were 5.0~120 ng/mL, 0.9974, and 2.1 ng/mL, respectively. For validating this proposed technique, the aqueous samples (stream water, reservoir water, and wastewater), the plastic sample and the diluted brass sample were used. Recovery yields of 93~102% were obtained. These measured data were not different from ICP-MS data at 95% confidence level. This method was also validated by the rice flour CRM (normal, fortified) samples. Based on the results from the experiment, it was found that this proposed technique could be applied to the determination of Cu(II) in various real samples.

• 분석과학
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• 제14권1호
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• pp.64-71
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• 2001

본 논문에서는 검출한계에 대한 기본개념을 기초로 백그라운드 측정시간과 시료측정시간을 고려한 검출한계치 유도과정을 기술하였다. 환경시료 중 Pu의 MDA값 결정에 영향을 미치는 여러인자들 중에서 시료량, 백그라운드 측정시간 및 시료측정시간 변화에 따른 MDA 변동값을 계산하였다. 환경시료에 대한 저준위 방사능 동위원소 측정시 본 연구결과를 통해 도출된 백그라운드 및 시료 측정시간의 적절한 배분에 의한 MDA 계산은 환경방사능 측정결과에 대한 신뢰도 평가에 활용이 가능하다.

• 분석과학
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• 제11권5호
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• pp.341-346
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• 1998

$Cu^{2+}$을 2-피리딘카르복살데히드(PyTC)와 반응시켜 $[Cu(PyTC)H_2O)]SO_4$를 얻었다. 이화합물은 1:1 전해질이며 물과 극성 유기 용매에 아주 잘 녹았다. 이 착물의 원소분석, 전기전도도 및 분광학적 데이터에서 이화합물의 구조는 사각평면임을 제시하였다. PyTC를 이용한 Cu(II)의 정량 가능성에 대하여 연구하였다. 구리(II)의 PyTC용액은 pH 4에서 $2.9{\times}10^{-4}M$까지 Beer의 법칙에 따랐다.

• 분석과학
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• 제8권3호
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• pp.273-279
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• 1995

납과 카드뮴을 포함하는 여러 가지 농도의 동결건조된 혈액이 외부정도관리 시료로서 제조되었다. 이 시료들은 흑연료 원자흡수분광법(GFAAS)을 이용하여 성능이 파악되었다. 매트릭스 개선제로서 0.1% ammonium dihydrogen phosphate와 0.1% Triton X-100을 사용하여 섭씨 600 내지 650도의 회화온도에서 혈액에 있는 납과 카드뮴의 정량 분석을 위한 GFAAS의 최적 분석조건이 얻어졌다. 제조된 혈액의 균질도와 안정도는 최적화된 분석조건에서 연구되었다.

• Bulletin of the Korean Chemical Society
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• 제24권3호
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• pp.285-290
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• 2003

An analytical method for the simultaneous determination of trace Ge, As and Se in biological samples by inductively coupled plasma/mass spectrometry has been investigated. The effects of added organic gas into the coolant argon gas on the analyte signal were studied to improve the detection limit, accuracy and precision. The addition of a small amount of methane (10 mL/min.) into the coolant gas channel improved the ionization of Ge, As and Se. The analytical sensitivity of the proposed Ar/CH₄system was superior by at least two-fold to that of the conventional Ar method. In the present method, the detection limits obtained for Ge, As and Se were 0.014, 0.012 and 0.064 ㎍/L, respectively. The analytical reliability of the proposed method was evaluated by analyzing the certified standard reference materials (SRM). Recoveries of 99.9% for Ge, 103% for As, 96.5% for Se were obtained for NIST SRM of freeze dried urine sample. The proposed method was also applied to the biological samples.