• 분석과학
• /
• 제8권3호
• /
• pp.391-396
• /
• 1995

A rapid preconcentration method based on solvent extraction is described for the determination of gold by flame atomic absorption spectrophotometry. Trace amounts of gold was extracted as a new chelating agent, 3-thiophenaldehyde-4-phenyl-3-thiosemicarbazone from pH 4.0 in diisobutyl ketone. The method is simple, fast, free from the effect of many interfering ions and has a high sensitivity and a good precision. Gold is quantitatively separated and concentrated from the elements in standard sample, and the value of the recovery was 91.7 and 108.3% by the proposed method.

• 대한화학회지
• /
• 제29권3호
• /
• pp.220-225
• /
• 1985

불꽃 원자 흡수 분광법의 Micro Sampling Technique을 이용하여 염의 농도가 높고, 양이 제한된 시료중에 미량으로 함유된 Cu, Zn 및 Fe의 분석을 시도하였다. 최적기간 및 분석조건을 조사한 결과 측정시간 0.3초, 시료부피 100${\mu}l$, 시료의 흡입속도 7.5ml/min, 연료와 산화기체의 혼합비 2.0 및 버어너 높이는 Cu일때 6.0mm, Zn 및 Fe는 8.0mm이었다. 이 방법을 일반적인 불꽃 방법과 비교하여 보면 시료의 전처리 과정이 필요없이 간단하고, 비교적 정밀성과 정확성이 있으며, 특히 100${\mu}l$정도로 양이 제한된 시료와 약 20% 정도로 염의 농도가 높은 시료의 경우도 버어너 틈새가 막히지 않고 안정한 불꽃에서 분석이 가능하였다.

• Journal of Preventive Medicine and Public Health
• /
• 제17권1호
• /
• pp.269-279
• /
• 1984

The optimum conditions for measuring cadmium content of less than 0.2ppm by flame atomic absorption spectrophotometry were investigated. The cadmium in urine was extracted by APDC-MIBK for the analysis by atomic absorption spectrophotometry after ashing them by a wet method. 1. Optimum conditions by APDC-MIBK and DDTC-MIBK extractions. The acidic aqueous solution was prepared with appropriate amount of 0.IN nitric acid, 5ml of 25% (W/V) sodium potasstum tartarate, 10ml of saturated ammonium sulfate, and 2ml of 2% APDC(or 1 ml of 5% DDTC) chelating agent. The total volume of solution was adjusted to 55 ml and pH to $2{\sim}10$ (or$7{\sim}10$). The aqueous solution was extracted with 10ml MIBK. Concentration of Triton X-100 did not effect the absorbance for APDC-MIBK extraction of cadmium, but absorbance decreased as the concentration increased for DDTC-MIBK extraction. The sensitivity and detection limits for the cadmium determination from APDC-MIBK extraction were 0.0038ppm and 0.0102, 0.0022ppm and 0.0116 for DDTC-MIBK, and 0.0132ppm and 0.0034 for 0.1N nitric acid. APDC-MIBK and DDTC-MIBK extractions were 3 times higher than 0.1N nitric acid for the sensitivity. 2. Excretion of cadmium in 24-hour urine by APDC-MIBK extraction. Determination of cadmium in urine by atomic absorption spectrophotometry of A.A. (Cd=2 mA) mode and B.C. (Cd=4 mA) mode and B.C. (Cd=4mA, $D_2=20mA$) mode showed some difference (p<0.05). The difference of cadmium determination and recovery according to method of standard additions and standard calibration curve method in urine was not significant (p>0.05, $93.48{\pm}11.78%,\;94.83{\pm}22.00%$). Excretion of cadmium in 24-hour urine collection from normal person and variance analysis within measurement variation was not significant (p>0.05), but between interindividual was significant (0.05). Determination of cadmium content by two different methods of flame atomic absorption spectrophotometry and dithizone colorimetry showed that the results from the two methods can be described by a regression line with a good correlation (y=1.0153x-0.2927, x=Cd by D.C., y=Cd by A.A.S., $r=0.8651^*$, p<0.01).

• 한국해양학회지
• /
• 제15권1호
• /
• pp.66-70
• /
• 1980

A method for the determination of dissolved species of Cd, Co, Cu, Ni, Pb and Zn in sea water by flame atomic absorption spectrophotometry (AAS) is described. Prior to analysis by AAS, these elements are concentrated by coprecipitation with iron pyrrolidinedithiocarbamate at pH 3 because of matrix effects and their low concentration levels in sea water. The detection limits are 0.01, 0.04, 0.02, 0.05, 0.08, and 0.03$\mu\textrm{g}$/l, and the relative standard deviations are 1.0, 2.4, 1.3, 2.9, 2.0 and 2.9% for Cd, Co, Cu, Ni, Pb and Zn, respectively. The method is shown to be satisfactory in terms of recovery and precision for the determination of these metals in sea water.

• Journal of Microbiology and Biotechnology
• /
• 제26권5호
• /
• pp.846-853
• /
• 2016

We displayed four types of Solanum nigrum metallothionein (SMT) for the first time on the surface of Saccharomyces cerevisiae using an α-agglutinin-based display system. The SMT genes were amplified by RT-PCR. The plasmid pYES2 was used to construct the expression vector. Transformed yeast strains were confirmed by PCR amplification and custom sequencing. Surface-expressed metallothioneins were indirectly indicated by the enhanced cadmium sorption capacity. Flame atomic absorption spectrophotometry was used to examine the concentration of Cd²⁺ in this study. The transformed yeast strains showed much higher resistance ability to Cd²⁺ compared with the control. Strikingly, their Cd²⁺ accumulation was almost twice as much as that of the wild-type yeast cells. Furthermore, surface-engineered yeast strains could effectively adsorb ultra-trace cadmium and accumulate Cd²⁺ under a wide range of pH levels, from 3 to 7, without disturbing the Cu²⁺ and Hg²⁺. Four types of surfaceengineered Saccharomyces cerevisiae strains were constructed and they could be used to purify Cd²⁺-contaminated water and adsorb ultra-trace cadmium effectively. The surface-engineered Saccharomyces cerevisiae strains would be useful tools for the bioremediation and biosorption of environmental cadmium contaminants.

• 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.

• Bulletin of the Korean Chemical Society
• /
• 제17권4호
• /
• pp.338-342
• /
• 1996

A sensitive method for the determination of trace cadmium after the preconcentration by extracting its 8-hydroxyquinoline complex into a molten benzophenone was developed. Several experimental conditions such as the pH of solution, the amounts of 8-hydroxyquinoline and benzophenone, stirring time, and standing time were optimized. Trace cadmium in 100 mL water sample was chelated with 2.5 mL of 0.001 M 8-hydroxyquinoline at pH 8.0. After 0.07 g benzophenone was added, the solution was heated to about 70 ℃ and stirred vigorously for 1 minute to dissolve the complex quantitatively in a molten benzophenone, and stood for 30 minutes to reproduce the microcrystalline benzophenone. The benzophenone containing Cd-8-hydroxyquinoline complex was filtered and dissolved in acetone. Cadmium was determined by a flame atomic absorption spectrophotometry. The interfering effects of diverse concomitant ions were investigated and eliminated. This method could be applied to natural water samples and the recovery of more than 90% was obtained in the real samples.

• Bulletin of the Korean Chemical Society
• /
• 제23권6호
• /
• pp.861-865
• /
• 2002

A sensitive method for the determination of trace copper(II) after the preconcentration by adsorbing its cupferron complex onto microcrystalline benzophenone was developed.Several experimental conditions such as the pH of sample solution,concentration of cupferron, amount of benzophenone and atirring time were optimized. Trace compper(II) in 100mL solution was chelated with $3.0\;{\times}\;10^3$ M cupferron at pH 5.0. After 0.20g benzophenone, The benzophenone adsorbing Cu-cupferron complex was filtered and then Cu-cupferron complex was desorbed in 10 mL ethanol. Copper was determined by a flame atomic absorption spectrophotomethry. The interfering effects of diverse concomitant ions were investigated. Fe(III) interfered seriously with, but the interference by Fe(III) was completely eliminated by adjusting the concentration of copferron to $5.0\;{\times}\;10^3$ M. The detection limit of this method was 8.6${\times}$10 M(5.5 ngmL$^1$). Recoveries of 97% and 96% were obtained for Cu(II) in a stream water and a brass sample, respectively. Based on the results from the experiment. this proposed technique could be applied to the determination of copper(II) in real samples.

• Bulletin of the Korean Chemical Society
• /
• 제28권8호
• /
• pp.1375-1382
• /
• 2007

A column preconcentration method with pulverized Amberlite XAD-4 loaded with bismuthiol I (BI) has been developed for the determination of trace Cd(II) and Cu(II) in various real samples by flame atomic absorption spectrophotometry. Various experimental conditions, such as the size of XAD-4, adsorption flow rate, amount of bismuthiol I, stirring time for adsorbing bismuthiol I on XAD-4, pH of sample solution, amount of XAD-4- BI, desorption solvent, and desorption flow rate, were optimized. Also, the adsorption capacity and the adsorption rate of Cd(II) and Cu(II) on XAD-4-BI were investigated. The interfering effects of various concomitant ions were investigated, Bi(III), Sn(II) and Fe(III) were found to affect the determination. But the interference by these ions was completely eliminated by adjusting the amount of XAD-4-BI resin to 0.70 g, although the adsorption flow rate was slower. For Cd(II) our proposed technique obtained a dynamic range of 0.5-40 ng mL-1, a correlation coefficient (R2) of 0.9913, and a detection limit of 0.3 ng mL-1. For Cu(II), the corresponding values were 2.0-120 ng mL-1, 0.9921 and 1.02 ng mL-1. To validate this proposed technique, the aqueous samples (stream water, reservoir water, tap water and wastewater), the diluted brass sample and the plastic sample, as real samples, were used. Recovery yields of 91-103% were obtained. These measured data were not different from ICP-MS data at 95% confidence level. Our proposed method was also validated using rice flour CRM (normal, fortified) samples. From the results of our experiment, we found that the technique we present here can be applied to the determination of Cd(II) and Cu(II) in various real samples.

• Bulletin of the Korean Chemical Society
• /
• 제20권4호
• /
• pp.431-435
• /
• 1999

An organic precipitate flotation of Cd(Ⅱ) and Pb(Ⅱ) was investigated by the coprecipitation with lanthanum 8-hydroxyquinolinate. Trace amounts of Cd(Ⅱ) and Pb(Ⅱ) with a significantly large amount of La(Ⅲ) were simultaneously precipitated in a 1,000 mL sample solution with the ethanolic 8-hydroxyquinoline solution. The pH was adjusted to 9.0 with 2 M ammonia solution. The precipitates were floated with the aid of tiny nitrogen bubbles and supported by the stable foam layer of sodium lauryl sulfate. The floats were collected on the fritted glass filter by a suction. The material collected was dissolved with 5.0 mL of ethanol and 1.5 mL of concentrated nitric acid, and then diluted to 25.0 mL with a deionized water. The analytes were determined by a flame atomic absorption spectrophotometry. The recoveries of the analytes spiked in the sample were 94.8% for Pb(Ⅱ) and 92.0% for Cd(Ⅱ). This flotation technique is simple and rapid, and also applicable to the determination of trace Cd(Ⅱ) and Pb(Ⅱ) at lew ppb levels.