• Bulletin of the Korean Chemical Society
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• 제27권11호
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• pp.1780-1784
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• 2006

Cloud point extraction was used to extract mefenamic acid (MF) from human urine, and spectrofluorimetry and spectrophotometry were used to analyze extracted MF. The variables affecting extraction and phase separation, i.e. HCl and Triton X-114 concentration, temperature and time of equilibration, were optimized. Under the experimental conditions used the limit of detection for extraction of 25 mL of sample was 0.006 and 0.045 mg $L^{-1}$, with relative standard deviations of 2.52 and 1.45% (n = 5) for spectrofluorimetric or spectrophotometric methods, respectively. Good recoveries in the range of 95-107% were obtained for spiked samples. The proposed methods were applied to the determination of MF in human urine.

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

• 분석과학
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• 제8권3호
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• pp.391-396
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• 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.

• 한국수산과학회지
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• 제9권3호
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• pp.169-175
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• 1976

해수중 ppb 정도의 카드뮴, 구리, 납, 아연 및 수은 정량을 위한 용매추출-원자흡광법 및 환원기화법에 의한 무염원자흡광법을 검토했다. 용매추출 때의 최적 pH는 pH4-7였으며 용매로는 MIBK가 가장 효율이 좋았으며 킬레이트제로는 DDTC가 APDC보다 추출율 및 기타 조건이 유리했다. 즉 $1\iota$ 해수를 사용하여 pH4-5에서 DDTC-MIBK로 추출하여 아세칠렌-공기불꽃 중에 흡입시켜 흡광도를 측정하는 방법으로 해수시료를 분석한 결과 정밀저는 표준편차로 카드뮴 0.058 ppb, 구리 0.084 ppb, 납 0.44ppb였다, 아연은 $1\iota$ 시수를 사용했을 때는 블랭크값이 녀무 크게 나오고 그 정밀도가 극히 좋지 않았다. 시수량을 200ml로 했을 때는 비교적 정밀도가 좋았으며 표준편차로서 2.49 ppb였다. 수은은 시수 500ml을 황산-과망간산칼리움 분해법으로 분해시켜 염화제1주석으로 수은을 환원기화시켜 흡광도를 측정했으며 그 정밀도는 0.005 ppb였다. 이상의 방법으로 측정할 수 있는 각 금속의 정량감도는 카드뮴 $0.08\;ppb/\%$, 구리$0.15\;ppb/1\% $, 납 $0.6\;ppb/1\%$, 아연 $1.2\;ppb/1\%$, 수은 $0.01\;ppb/1\%$였다. 채수후 분석시까지의 시수보관에 따른 각 금속의 농도변화는 시수$1\iota$에 대해 질산 10ml 정도 넣어 pH 1.5 부근으로 하며 플리에칠렌병에서 보관한 결과 카드뮴, 구리, 납, 수은은 30일정도 까지는 안정하였으며 아연은 불규칙한 심한 변동을 보였다.

• Bulletin of the Korean Chemical Society
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• 제28권3호
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• pp.373-378
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• 2007

A micro organism Agrobacterium tumifacient as an immobilized cell on a solid support was presented as a new biosorbent in a simple and sensitive spectrophotometry determination of Ni(II) in various samples using 4-hydroxy benzaldehyde-4-bromophenyl hydrazone as a color developing agent (λmax 497 nm) at pH 4.0 ± 0.2. Beer's law was obeyed over the range of 0.01-0.1 μg L-1. The molar absorptivity and Sandell's sensitivity were 1.285 × 105 L mol-1cm-1 and 0.007245 μg cm-2 respectively. Under these conditions, the preconcentration factor obtained was 82, and the detection limit achieved was 0.05 μg L-1. The detailed study of various interfering ions made the method more sensitive and selective. The recovery of Ni(II) from various samples range from 97.75 to 99.35%. The present method was successfully applied for the determination of Ni(II) in spiked, natural water and alloy samples. The proposed method was compared with reported methods in terms of Student's ‘t'-test and Variance ratio ‘f'-test which indicates that there is no significant difference between proposed and literature method at 95% confidence level.

• 대한임상검사과학회지
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• 제40권2호
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• pp.113-117
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• 2008

It designed a study to examine the efficiency of DNA and RNA extraction from archival formalin-fixed, paraffin-embedded tissues using an non-heating and heating method. Archival paraffin blocks of liver, kidney, colon were randomly selected. Each paraffin block was prepared in 20 microtubes. For each paraffin blocks were tested non-heating DNA extraction to 10 microtubes and heating protocol under pH 7.0 and $100^{\circ}C$ to 10 microtubes. Evaluation of the results of DNA extraction was carried out by measuring concentration by UV spectrophotometry and then PCR amplification. DNA extraction content that non-heating method was liver $5{\pm}0.7{\mu}g/mL$, kidney $2{\pm}0.3{\mu}g/mL$, colon $6{\pm}0.4{\mu}g/mL$ and heating method was liver $12{\pm}0.6{\mu}g/mL$, kidney $7{\pm}0.5{\mu}g/mL$, colon $10.{\pm}0.3{\mu}g/mL$. Successful RNA extraction was observed, by ${\beta}$-actin amplification, in 46.7% sections for samples treated by the heating method versus 30.0% using non-heating DNA extraction. The extracted nucleic acid showed better values for samples heated at $100^{\circ}C$. Therefore heating extraction of nucleic acid is reliable, quick and efficiency.

• 분석과학
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• 제15권1호
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• pp.72-79
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• 2002

Di-(2-ethylhexyl)phthalate (DEHP) 가 가소제로 첨가되 있는 poly(vinylchloride) (PVC) 제품의 사용중에는 DEHP가 방출되어 나올 가능성이 있다. 이때 추출되는 DEHP의 정량적인 측정법에는 여러가지가 있으나 그 방법에 따라 용출량에 많은 차이가 발생하기 때문에 측정방법과 결과에 대한 비교분석은 시급한 과제라 할 수 있다. 이를 평가하기 위하여 PVC를 주원료로 하는 혈액백과 수액백에서의 DEHP 용출에 관한 연구를 기체 크로마토그래프와 분광광도계를 이용한 두 가지 방법으로 수행하였다. 5종류의 PVC 백을 실험 재료로 선택하여 $40{\times}10{\times}0.4mm$ 크기의 시편을 제조하고 이를 용출액에 담가 1시간동안 DEHP를 용출하였다. 기체 크로마토그래프로 DEHP 를 검출한 결과 시료에 따라 $23.2{\sim}70.9{\mu}g/mL$ 의 DEHP가 용출되는 것을 알 수 있었다. 반면 PVC백 안에 용출액을 주입하여 1시간 동안 DEHP를 용출시키고 분광 광도계를 이용하여 DEHP를 검출한 결과 $24.8{\sim}41.3{\mu}g/mL$의 DEHP가 용출되었다. 용출 조건과 실험방법에 따라 서로 다른 수치를 보임을 알 수 있었고 단위 시간 단위 면적 당 용출되는 DEHP의 양은 일정하다는 전제 하에 두 실험의 결과를 비교하고 환산하는 식을 구하여 적용한 결과 두 측정방법에서 얻어진 용출량이 거의 일치하였다.

• Nuclear Engineering and Technology
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• 제32권4호
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• pp.309-315
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• 2000

The changes of Np oxidation state in nitric acid and the effect of nitrous acid on the oxidation state were analyzed by spectrophotometry, solvent extraction, and electrochemical methods. An enhancement of Np extraction to 30 vol.% TBP was carried out through adjustment of Np oxidation state by using a glassy carbon fiber column electrode system. The information of electrolytic behavior of nitric acid was important because the nitrous acid affecting the Np redox reaction was generated during the electrolytic adjustment of the Np oxidation state. The Np solution used in this work consisted of Np（V) and Np（Ⅵ）without （IV）. The composition of Np（V) in the range of 0.5M -5.5 M nitric acid was 32% ~ 19%. The electrolytic oxidation of Np（V) to Np（Ⅵ）in the solution enhanced Np extraction efficiency about five times higher than the case without the electrolytic oxidation. It was confirmed that the nitrous acid of less than about 10-5 M acted as a catalyst to accelerate the chemical oxidation reaction of Np（V) to Np（Ⅵ）.

• 약학회지
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• 제8권4호
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• pp.96-99
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• 1964

In the previous study, the composition ratios of the Cu-sulfa drugs complexes determined by gravimetric and solvent extraction method reported. In this paper, the continuous variations method has been used to know whether the complexes are simple complexes or chelates, and to recertify the composition ratios of the complexes at pH 7-8. It has been certified that the ratio of $Cu^{+2}$ ion to sulfa drugs in 1:2 from the result of this experiment.

• Bulletin of the Korean Chemical Society
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• 제25권4호
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• pp.545-548
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• 2004

A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with $C_{18}$ membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with $C_{18}$ membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was $1.32{\times}10^5L\;mol^{-1}cm^{- 1}$ at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 ${\mu}$g/mL. This method was applied to the determination of nickel in water and biological samples with good results.