• 분석과학
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• 제20권3호
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• pp.183-192
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• 2007

최근의 전기전자제품 중 유해물질규제지침(RoHS)이나 폐전기전자제품 처리 지침(WEEE) 등의 각종 환경규제는 국제교역에 있어 실질적인 무역장벽으로 작용하고 있다. 한국표준과학연구원(KRISS)에서는 이와 같은 환경규제와 관련하여 국내시험연구기관 및 관련산업체실험실의 측정 신뢰성 확보를 위한 숙련도 시험을 실시하였다. 참여기관은 국내 전기전자 제품 및 자동차 관련 실험실 31개소이다. 숙련도시험용 시료는 pellet type 폴리프로필렌 소재 2 종이며, 측정대상원소는 유럽공동체의 RoHS 지침에서 규정하고 있는 6개 성분 중 카드뮴 (Cd)과 납 (Pb)이다. 시료는 2006년 9월 1일 각 참여실험실에 우편 송부하였으며 10월 10일까지 측정 결과를 접수하였다. 각 실험실의 측정 결과는 KRISS 기준값과의 비교, Robustic Z-score, Youden plot 등에 의해 비교 평가하고 전처리 방법에 따른 측정 결과도 비교 검토하였다. 전반적으로 기준값과의 10% 범위 내에서 일치되는 결과를 보고하였으나 일부 실험실은 심각한 bias를 보이고 있어 측정결과의 신뢰성 향상을 위한 품질보증 시스템을 갖추어야 할 필요가 있다.

• 한국축산식품학회지
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• 제28권3호
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• pp.301-305
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• 2008

조제분유중의 요오드 및 염소를 신속하고 정확하게 분석하기 위해 이온선택성 전극을 이용한 분석을 실시하였다. 전극을 이용한 측정시 영향을 주는 간섭물질을 제거하기 위해 시료를 용해한 후 3% 아세트산 2 mL를 투입하고, 정제는 filter paper(No.541, Whatman, UK)를 이용하여 여과하는 방법을 선택하였다. 요오드 및 염소이온이 pH에 의해 영향을 받는 것을 확인할 수 있었으며, 0.1 N NaOH를 사용하여 pH를 7.0으로 보정하여 농도를 측정함으로써 요오드와 염소의 회수율 각각 $93.7{\pm}2.7%$와 $103.9{\pm}4.9%$의 결과를 얻을 수 있었다. 간단하고 신속한 간섭물질 제거와 정제를 통해 조제분유중의 요오드 및 염소이온의 농도를 이온전극으로 신속하고 정확하게 측정할 수 있었다.

• Journal of Radiation Protection and Research
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• 제36권4호
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• pp.223-229
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• 2011

일반적으로 사용되는 액체섬광계수기를 이용한 $^{226}Ra$ 분석에는 Ba 공침법을 통해 얻어진 $Ba(Ra)SO_4$ 침전물을 이용하게 된다. 그러나, 인산석고 침출수의 경우 ${SO_4}^{2-}$, $Ca^{2+}$등의 이온이 다량 존재하여 순수한 $Ba(Ra)SO_4$ 침전물을 얻기가 힘들기 때문에 정확한 분석이 매우 어렵다. 본 연구에서는 분석화학에서 금속이온의 분리에 일반적으로 많이 활용되는 Ethylenediaminetetraacetic acid (EDTA)를 이용하여 인산석고 침출수에서의 Ba 공침법을 개발하였고 실제 인산석고 야적장 주변 침출수의 분석에 적용하였다. 또한 개발된 분석 방법은 침출수와 유사한 매질의 $^{226}Ra$ 모의표준시료을 제조하여 확인하였고 IAEA-434 인증표준물질을 통해 분석 신뢰성을 검증하였다. 실제 인산석고 야적장 침출수를 분석한 결과 0.102 $Bq{\cdot}kg^{-1}$의 농도를 보였고 검출하한치는 3.4 $mBq{\cdot}kg^{-1}$였다. $^{226}Ra$ 모의표준시료 분석을 통한 측정농도는 첨가한 농도와 1% 내외로 잘 일치하며 좋은 상관관계($R^2$=0.99)를 보였다. 인증표준물질의 분석 결과 인증값과 비교하여 5.8% (k=1)이내로 잘 일치하였다.

• 분석과학
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• 제28권6호
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• pp.460-466
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• 2015

분유 내 콜레스테롤을 정량분석하기 위한 일차분석법으로 동위원소희석 질량분석법을 개발하였다. 내부표준물질로 콜레스테롤-d₄를 사용하여 분유에 첨가하였다. 분유에 지방산과 에스테르형태로 결합되어 있는 콜레스테롤을 자유 콜레스테롤로 바꾸어주기 위해 비누화과정을 수행하였다. 비누화과정은 반응온도, 반응시간, 사용한 KOH의 농도에 따라서 최적화하였으며, 그 결과로 분유시료 0.1 g에 대해 70 ℃에서 180 분 동안 8 M의 KOH 0.8 mL를 첨가하여 반응을 진행시키는 최적화조건을 확립하였다. 이와 같은 조건으로 실험을 진행하여 재현성은 0.23%, 확장불확도는 95%의 신뢰범위에서 1.9%로 추정되었다. 확립된 동위원소희석 질량분석법의 유효화를 위해 분유내에서 콜레스테롤의 인증값을 가지는 NIST SRM을 측정하였고 이 결과가 인증값과 불확도 범위내에서 일치하는 것을 확인하였다.

• 한국세라믹학회지
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• 제51권5호
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• pp.472-476
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• 2014

In this work, a new method that utilizes L-cysteine salicylaldehyde Schiff-base modified macroporous polystyrene resin (PS-CSC) as an effective sorbent has been developed for preconcentration of trace cadmium and lead in environmental water samples. The effect of pH, the contact time, the elution conditions, the flow rate, the initial concentration of target metal ions, and the effects of interfering ions on the preconcentration of the analytes were investigated. The maximum adsorption capacity of PS-CSC under optimum conditions for cadmium and lead were found to be 6.03 - 18.17 mg/g and 12.58 - 36.13 mg/g when the initial concentration of metal ions between 5.0 - 90 mg/L. The limits of detection for cadmium and lead were 2.46 ng/L and $0.52{\mu}g/L$, with a preconcentration factor of 200. The developed method has been validated by analyzing certified reference material and successfully applied for the enrichment and determination of trace cadmium and lead from environmental water samples.

• Bulletin of the Korean Chemical Society
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• 제31권7호
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• pp.1907-1914
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• 2010

A novel catalytic kinetic method is proposed for the determination of Se(IV), Se(VI) and total inorganic selenium in water based on the catalytic effect of Se(IV) on the reduction of bromate by p-nitrophenylhydrazine at pH 3.0. The generated bromine, $Br_2$ or $Cl_2$ plus $Br_2$ in 0.1 M NaCl (or NaBr) environment efficiently decolorized Calmagite and the reaction was monitored spectrophotometrically at 523 nm as a function of time. In this indicator reaction, bromide acted as an activator for the catalysis of selenium (IV) and a reducing agent for selenium (VI) at pH 3.0, which allowed the determination of total selenium. The fixed time method was adopted for the determination and speciation of inorganic selenium. Under the optimum conditions, the calibration graph are linear in the range 1 - 35 ${\mu}gL^{-1}$ of Se(IV) for the fixed time method at $25^{\circ}C$. The detection limit based on statistical $3S_{blank}$/m-criterion was 0.215 ${\mu}gL^{-1}$ for the fixed time method (7 min). All of the variables that affect the sensitivity at 523 nm were investigated, and the optimum conditions were established. The interference effect of various cations and anions on the Se (IV) determination was also studied. The selectivity of the selenium determination was greatly improved with the use of the strongly cation exchange resin such as Amberlite IR120 plus. The proposed kinetic method was validated statistically and through recovery studies in natural water samples. The RSDs for ten replicate measurements of 5, 15 and 25 ${\mu}gL^{-1}$ of Se(IV) and Se(VI) was changed between 2.1 - 4.85%. Analyses of a certified standard reference material (NIST SRM 1643e) for selenium using the fixed-time method showed that the proposed kinetic method has good accuracy. Se(IV), Se(VI) and total inorganic selenium in environmental water samples have been successfully determined by this method after selective reduction of Se(VI) to Se(IV).

• 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.

• 한국환경보건학회:학술대회논문집
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• 한국환경보건학회 2003년도 Challenges and Achievements in Environmental Health
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• pp.177-180
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• 2003

A glassy carbon electrode(GCE) modified with nafion-DTPA-glycerol was used for the highly selective and sensitive determination of a trace amount of Cu$\^$2+/. Various experimental parameters, which influenced the response of nafion-DTPA-glycerol modified electrode to Cu$\^$2+/, were optimized. The copper(II) was accumulated on the electrode surface by the formation of the complex in an open circuit, and the resulting surface was characterized by medium exchange, electrochemical reduction, and differential pulse voltammetry, A linear range was obtained in the concentration range 1.0${\times}$10$\^$-8/M∼1.0${\times}$10$\^$-6/M Cu(II) with 7 min preconcentration. Further, when an approximate amount of lead(II) is added to the test solution, nafion-DTPA-glycerol modified glassy carbon electrode has a dynamic range of 2 orders magnitude(1.0${\times}$10$\^$-9/M∼1.0${\times}$10$\^$-7/M). The detection limit(3 $\sigma$) was as low as 5.0${\times}$10$\^$-6/M(0.032ppb). The interferences from other metal ions could be reduced by adding KCN into the sample solutions. This method was applied to the determination of coppe,(II) in certified reference material(3.23${\times}$10$\^$-7/M, 21ppb), sea water(9.50${\times}$10/sup-7/M, 60ppb). The result agrees satisfactorily with the value measured by Korea Research Institute of Standard and Science.

• 대한수의학회지
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• 제52권2호
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• pp.69-74
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• 2012

The analytical method of trace toxic metals in livestock products was confirmed and validated through certified reference material (CRM) and the international proficiency tests. There are some difficulties to determine low levels of toxic metals in livestock products because of interferences due to the matrix. The recoveries of CRM (NIST 1577c) ranged from 73.9 to 119% for lead and from 86.4 to 111% for cadmium in bovine liver. The international proficiency tests were carried out with the milk powder and cocoa powder samples including metals provided by Food Analysis Performance Assessment Scheme (FAPAS$^{(R)}$, UK). The test samples were prepared by microwave digestion using solution of $HNO_3:H_2O_2:H_2O$ (v/v/v = 5 : 2 : 4) and analyzed by ICP/MS. The analytical result of cadmium in milk powder was $121{\mu}g/kg$ with -0.3 of the z-score compared to the assigned value of $131{\mu}g/kg$ by FAPAS$^{(R)}$. The analytical results of lead and cadmium in cocoa powder were $29.2{\mu}g/kg$ and $97.6{\mu}g/kg$, respectively, which satisfied the assigned values of $34.2{\mu}g/kg$ for lead and $126{\mu}g/kg$ for cadmium by FAPAS$^{(R)}$. It is verified that the analytical method is accurate and reliable to determine trace lead and cadmium in livestock products by microwave digestion and ICP/MS.

• 농업과학연구
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• 제46권2호
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• pp.315-322
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• 2019

In this study, the contents of ${\beta}$-carotene and cholesterol were evaluated in various types of agricultural and processed foods (vegetables, legume products, dairy products, and eggs). Certified reference material (CRM) with an assigned value was used for the validation of the ${\beta}$-carotene and cholesterol analytical methods. High recoveries (accuracy) of ${\beta}$-carotene (96%) and cholesterol (97%) were obtained from the quantitative analysis of the CRM, with a relative standard deviation (%) of 1.86 and 3.35% for the ${\beta}$-carotene and cholesterol, respectively. Vegetables contained relatively high concentrations of ${\beta}$-carotene (raw Toona sinensis, $1650.97{\mu}g/100g$, a raw small onion, $879.09{\mu}g/100g$, and a raw lettuce stem, $591.89{\mu}g/100g$). The ${\beta}$-carotene values in dried chickpeas ($22.94{\mu}g/100g$) and dried brown lentils ($21.98{\mu}g/100g$) were similar. The highest ${\beta}$-carotene value among the analyzed dairy products was found in banana milk ($234.21{\mu}g/100g$) while other flavored products (strawberry milk and chocolate milk) did not contain any ${\beta}$-carotene. Furthermore, ${\beta}$-carotene was not detected in goat milk and high calcium milk in this study. With regard to cholesterol among the analyzed samples, the highest cholesterol value was found in egg yolk (629.30 mg/100 g), and cooking methods (boiling and frying) had little effect on the cholesterol levels of eggs. In addition, the cholesterol content in vanilla ice cream was 28.77 mg/100 g which was the highest value among the analyzed dairy products.