• Bulletin of the Korean Chemical Society
• /
• 제25권8호
• /
• pp.1125-1129
• /
• 2004

This work assesses the potential of natural Analcime Zeolite as an adsorbent for preconcentration of lead (II) traces. Lead is quantitatively retained on 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol by column method with Analcime in the pH range of 5-6.5 and 2 mL $min^{?1}$ flow rate. Lead was removed from the column with 10.0 mL of 4 M hydrochloric acid and was determined by anodic stripping differential pulse voltammetry. 0.5ppb detection limit was obtained and linear dynamic range was 3 to $1.2{\times}10^5$ ppb in final solution with correlation coefficient of 0.999 and relative standard deviation of ${\pm}$ 1.2% (for eight replicate determination of 2.5 ${\mu}g\;mL^{?1}$ of lead). Various parameters such as the effect of pH, flow rate, instrumental conditions and interferences of some ions on the determination of lead have been studied in detail for optimization of conditions. The method was successfully applied for determination of lead in various samples.

• Journal of Industrial and Engineering Chemistry
• /
• 제67권
• /
• pp.461-468
• /
• 2018

A highly sensitive, selective and rapid method for the determination of lead based on the reaction of lead (II) with 5-(4'-chlorophenylazo)-6-hydroxypyrimidine-2,4-dione (CPAHPD) and the solid phase extraction of the Pb(II)-CPAHPD complex with Amberlite XAD-2000 was developed, in the presence of pH 5.6 buffer solution and Triton X-114 medium. CPAHPD reacts with lead to form a violet complex with a molar ratio of 2:1 (CPAHPD to lead). This complex was enriched by the solid phase extraction with Amberlite XAD-2000. An enrichment factor of 500 was obtained by elution of the complex from the resin with a minimal amount of isopentyl alcohol(0.2 mL). In isopentyl alcohol medium,the molar absorptivity of the complex is $1.13{\times}10^6L\;mol^{-1}cm^{-1}$ at 647 nm. Beer's law is obeyed in the range of $5.0-160ng\;mL^{-1}$ in the measured solution. The relative standard deviation for 10 replicate samples of $50ng\;mL^{-1}$ level is 1.26%. The detection and quantification limits reaches 1.5 and $4.7ng\;mL^{-1}$ in the original samples. The presented procedure was successfully applied for determination of lead content in real samples such as vegetables, waters, biological and soil samples with satisfactory results.

• 한국환경보건학회:학술대회논문집
• /
• 한국환경보건학회 2003년도 Challenges and Achievements in Environmental Health
• /
• pp.204-207
• /
• 2003

Determination of Lead(II) using nafion-DTPA (diethylene triamine pentaacetic acid)-glycerol-modified glassy carbon electrodes is described. Lead(II) is accumulated at the electrode by complexing with the DTPA, reduced, and detected by differential pulse voltammetry. In this study, we demonstrate that at a preconcentration time of 5min the nafion-DTPA-glycerol-modified glassy carbon electrode has a linear calibration curve at range 1.0${\times}$10$\^$-9/M∼1.0${\times}$10$\^$-7/M in pH 4.0 buffer solution. The detection limit(3$\sigma$) is as low as 5.0${\times}$10$\^$-6/M. This method is applied to the determination of lead(II) in certified reference material and the result agrees satisfactorily with the certified value.

• 분석과학
• /
• 제10권4호
• /
• pp.240-245
• /
• 1997

ICP/MS에 의해 전혈 중의 납을 정확하게 분석하는 방법을 개발하였다. 전혈시료를 납의 오염과 손실 없이 마이크로파 분해장치에서 분해시키고, 96개 혈액시료 중의 $Pb^{208}$을 ICP/MS로 측정하여 분석하였다. 실제 인체 혈액 시료 중의 Pb 함량은 $2.50{\sim}22.8{\mu}g/dL$ 범위였다. NIST SRM 955a series를 분석함으로써 이 분석방법의 정확도를 확인하였다.

• 한국환경보건학회지
• /
• 제28권5호
• /
• pp.53-58
• /
• 2002

A method for the determination of lead(II) ion using a nafion-EDTA(ethylene diamine tetraacetic acid)-glycerol modified glassy carbon electrode was proposed. Lead(II) ion is accumulated at the electrode by complexation and electrostatic attraction with nafion-EDTA-glycerol and detected at -0.560$\pm$0.015V (vs. Ag/AgCl) by differential pulse voltammetry. For the determination of lead(II) ion, a standard calibration curve if obtained from 10$^{-9}$ M lead(II) ion to 10$^{-7}$ M, and the detection limit(3s) is as low as 5.0$\times$10$^{-10}$ M.

• Journal of Preventive Medicine and Public Health
• /
• 제7권2호
• /
• pp.377-381
• /
• 1974

Determination of lead in urine is important in industrial hygiene and toxicology. Dithizone method has been principally used for the determination of lead in urine, which gives accurate results in skilful hands but is usually complex and time-consuming. Atomic absorption spectrophotometry is a new simple method and several procedures have been described. However, the influences of pH and the presence of chelating agents during treatment of lead poisoning are not clear. The purpose of this study was to find out the effect of pH and chelating agents on the determination of lead using Shimadzu atomic absorption/flame spectrophotometer, model AA-610. The results obtained were as follows: 1. The atomic absorption spectrophotometry(AAS) could be applied without prior acid digestion to specimens in the absence of chelating agents. The absorbance at $2,170\;{\AA}$, though more sensitive, was more noisy electronically. Therefore, we selected the wavelength of $2,833\;{\AA}$ plus scale expansion. 2. The optimal pH was in the range from 2 to 3. 3. The sensitivity was $0.075{\mu}g/ml/%$ and detection limit was about $0.2{\mu}g/ml$. 4. In the presence of EDTA, lead could not be completely determined without prior acid digestion. 5. On specimens from patients receiving penicillamine therapy, a comparison was made between the values obtained with dithizone method and AAS method with prior acid digestion. The results of comparison showed a very good agreement.

• 대한화학회지
• /
• 제7권2호
• /
• pp.186-188
• /
• 1963

An attempt to improve the method of volumetric determination of tungsten developed by Luke has been made successfully. Using amalgam coated lead instead of pure metallic lead in the reduction procedure. W(VI)-W(III) reduction has been found to be quantitative in rather concentrated hydrochloric acid. Since there was no excessive dissolution of lead via reduction of hydrogen ion, lead surface was totally accessible for the reduction of tungsten and no trouble was caused by dereposition of $PbCl_2$ crystals at the nozzle of Jones reductor. Furthermore, it has been confirmed that almost 100 mg. of $WO_3$ can be handled easily if the chloride concentration of the HCl is increased by adding solid $NH_4Cl$.

• 한국환경보건학회지
• /
• 제2권1호
• /
• pp.29-31
• /
• 1975

This experiment Was carried out under two points of view, from May 1st to the end of 1973. One was the comparative determination of the activation factor of Lead dioxide by kinds in measuring of Sulfur oxides concentration by $PbO_2$ cylinder method, and the other was the comparison that result with the record of auto analyzer. Five measuring sites were selected out of Seoul City. Three kinds of Lead dioxide made in Japan (B,C and D) were compared with Standard $PbO_2$ (A for use in Determination of Sulphur in the atmosphere, purity 99% up) made in British Institution, and monthly measuring was conducted at every sampling site. The recording by auto analyzer (Beckman Model 906-A $SO_2$ Analyzer) was conducted once or twice a month for 24 hours at each sampling site during the same period. And some significant results were obtained. 1. In comparative experiments to determine the activation degree of three kinds of Lead dioxide (B,C and D), the obtained correction factor of B reagent was 1.09, 1.16 in C and 1.30 in D against Standard $PbO_2$ (A). Therefore, it should be in need of standardization or clear statement about the reagents for use, in determination sulfur oxides by $PbO_2$ cylinder method. 2. Generally, the concentration of Sulfur dioxide by wilkins' convertion method from $SO_3$ showed about 20-30% higher than those by Auto analyzer.

• 대한화학회지
• /
• 제13권4호
• /
• pp.313-316
• /
• 1969

모나자이트 중의 납함량을 신속하고 간편하게 결정하는 방법을 기술하였다. 즉 모나자이트 시료를 황산에 녹여 200ml가 되겠끔 희석하였다. 스트론튬으로 납을 정량적으로 분리한 후 3N 수산화나트륨에 녹였다. 여분의 Zn-EDTA를 가한 다음 남은 아연 이온을 0.01M EDTA표준용액으로 적정하였으며 이때 가리움제 (masking agent)러서 시안화칼륨 및 아세틸 아세톤을 가하였고 pH 5에서 자이렌을 오렌지(Xylenol orange)를 지시약으로 사용하였다.

• 대한화학회지
• /
• 제46권5호
• /
• pp.407-411
• /
• 2002

납이온과 선택적으로 상호작용하는 이온 운반물질(lead ionophore II)과 수소이온과 선택적으로 상호작용하면서 형광을 내는 변색성 이온 운반물질(ETH5294) 및 소수성의 음이온 자리를 포함하는 이온 선택성 광센서를 제조하여 형광분광법으로 수용액 중의 납이온을 정량하는 방법을 연구하였다. 시료용액의 pH,막두께 등이 형광세기에 미치는 영향을 조사하였다. $Na^+$, $K^+$, $Mn^{2+}$ 및 $Zn^{2+}$이온 등의 방해이온이 납이온의 정량에 미치는 영향을 조사하였다.본 연구에서 제작한 납이온 선택성 막을 이용하여 얻은 납이온 검정곡선의 직선범위는 5.0${\times}10^-7$M5.0${\times}10^-3$M이였고 이 범위에서의 상관계수는 -0099107이었다. 바탕용액의 상대표준편차는 3.0%였고 납이온의 검출한계는 5.0${\times}10^-9$M이었다.