• YAKHAK HOEJI
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• v.35 no.3
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• pp.182-189
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• 1991

Systematic study on the extraction of ion pair by the use of picric acid (PCA) as an ion pair forming reagent to the aliphatic amines has not be done by spectrophotometric method. The extraction of ion pair by the use of PCA and 23 kinds of the aliphatic amines was examined. The procedure is as follows; Elving's buffer solution (pH 1.3~10, ionic strength 0.5) each amine solution, and PCA solution were taken into a test tube. The mixture was shaken mechanically with chlorform. The organic phase was filtered through a filter paper to remove water droplets. The absorbance was examined at $\lambda_{max}$ against a reagent blank. Primary and secondary whose carbon number were more than 7 or 6, respectively, are extractable as ion pairs with PCA, while tertiary amines and quaternary ammonium salts are also extractable without the correlation of carbon number. It was considered that the ion pair extraction of primary and secondary amines was affected by the number of carbon of amines, but its extraction of tertiary amines or quaternary ammonium salts was affected by kind of aliphatic amines rather than pKa values or carbon number of amines.

• Archives of Pharmacal Research
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• v.13 no.2
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• pp.174-179
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• 1990

Second derivative (D2) spectrometry using ion-pair extraction technique was development for the determination of total glycyrrhetic acid (GA) in Glycyrrhizae Radix, Glycyr-rhizin (G) obtained from Glycyrrhizae Radix was hydrolyzed into GA in 2 N-HCI and methanol (1:1) and extracted from aqueous phase in the form of an ion-pair complex with tetrapentylammonium bromide (TPA) as a counter ion. Maximum D2 amplitude (Z value) was obtained when 1000-fold or greater molar ratio of TPA was used at pH 11. Reaction an effective extraction solvent of the ion-pair complex. The linearity of standard curve of ion-pair GA was obtained in the range of 4.120 $\mu$g/ml as GA. Assayed contents of GA in dry powder by D2 UV spectrometry and HPLC method were 5.31 $\pm$ 0.04% and 5.20 $\pm$ 0.008%, respectively.

• Bulletin of the Korean Chemical Society
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• v.23 no.10
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• pp.1381-1391
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• 2002

The solvent sublation using ion pairs of metal-2-naphthoate(2-HNph) and tetrabutyl ammonium ($TBA^+$) ion has been studied for the concentration and determination of ultra trace Bi(III), In(III) and Tl(Ⅲ) ions in water samples. The partition coefficients ($K_p$) and the extraction percentages of 2-HNph and the ion pairs to methyl isobutyl ketone (MIBK) were obtained as basic data. After the ion pair $TBA^+$·M$(Nph)_4^-$ was formed in water samples, the analytes were concentrated by the solvent sublation and the elements were determined by GF-AAS. The pH of the sample solution, the amount of the ligand and counter ion added and stirring time were optimized for the efficient formation of the ion pair. The type and amount of optimum surfactant, bubbling time with nitrogen and the type of solvent were investigated for the solvent sublation as well. 10.0 mL of 0.1 M 2-HNph and 2.0 mL of 0.1 M $TBA^+$ were added to a 1.0 L sample solution at pH 5.0. After 2.0 mL of 0.2%(w/v) Triton X-100 was added, the ion pairs were extracted into 20.0 mL MIBK in a flotation cell by bubbling. The analytes were determined by a calibration curve method with measured absorbances in MIBK, and the recovery was 80-120%.

• Journal of the Korean Chemical Society
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• v.27 no.6
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• pp.411-418
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• 1983

The effects of existing anions in hydrofluoric acid solutions, $F^-$ and $HF_2$on the extraction of methylene blue-$BF_4^-$ ion-pair into 1,2-dichloroethane have been investigated by spectrophotometry. The absorbance of the extracted ion-pair is found to be independent of $F^-$ion up to $10^{-2}$ molar concentration, which implies that $F^-$ion dose not directly interfere with the extraction. However, $HF_2^-$ ion competes with $BF_4^-$ion for methylene blue and the extraction constant for methylene blue-H$F_2$ion-pair is calculated to be 8.5 at $25^{\circ}C$.

• YAKHAK HOEJI
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• v.37 no.2
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• pp.119-123
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• 1993

A spectrophotomertic method is proposed for the determination of antihistamines. The method is based on solvent extraction of the ion pair formed between antihistamines and colored picric acid into chloroform. The binding state of antihistamines-picric acid complexes were presumed by IR and $^{1}$H-NMR spectra as intermolecular hydrogen bonding. This method was applicable to the determination of antihistamines in the pharamaceutical preparations.

• YAKHAK HOEJI
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• v.27 no.2
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• pp.125-131
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• 1983

Whether ($AB_{w}$) may be neglected against ($A_{w}^{+}$) in the calculation of the extraction coefficient of ion-pairs was criticized by both experiments and theoretical consideration, where ($AB_{w}$) and ($A_{w}^{+}$) mean the molar concentration of ion-pair AB and cation $A^{+}$ in the aqueous phase. Ion-pair complexes were partitioned between phosphate buffer (pH 7.4) and n-octanol. Tetrabutylammonium, isopropamide and methylene blue were selected as cations and benzoic acid, p-toluenesulfonic acid, salicylic acid and taurodeoxycholic acid were selected as counter ions (anions). As a result, conventional methods which assume no existence of ($AB_{w}$) were proven to lack generality. The equation proposed in my earlier report was confirmed to be valid as a general method.

• Journal of the Korean Chemical Society
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• v.26 no.5
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• pp.326-332
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• 1982

The structure of the complex extracted from an aqueous solution containing methylene blue and tetrafluoroborate with 1,2-dichloroethane has been investigated by comparing IR spectrum of the extract with those of pure components and appeared to be an 1 : 1 contact ion-pair between monovalent ions of opposite charge. The extraction constant obtained from the absorbance data measured at 658nm in 1,2-dichlorethane has a value of 1.1${\times}$at$10^4M{-1}$ 25$^{\circ}$C in the range from 1.43${\times}10^{-2}$ to 2.86${\times}10^{-1}$M HF. In the solvent extraction with nitrobenzene, the identical experiments show that extraction constants are increased with HF concentration possibly due to dissociation of the ion-pair in nitrobenzene.

• Bulletin of the Korean Chemical Society
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• v.22 no.8
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• pp.821-826
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• 2001

Solvent sublation has been studied for the separation and determination of trace Zn(Ⅱ) and Pb(Ⅱ) in water samples. A synergy producing method was utilized to improve the efficiency of extraction in the sublation using an ion-pair of metal-naphth oate {M-(Nph)3- } complexes and tetra-n-butylammonium (TBA+ ) ion. After the M-(Nph)3- complexes were formed by adding 1-naphthoic acid to the sample solution, tetra-n-butylammonium bromide was added in the solution to form the ion-pair. And sodium lauryl sulfate (SLS) was added to make the ion-pair hydrophobic. The ion-pairs of the metal complexes were floated and extracted into methylisobutyl ketone (MIBK) from the aqueous solution by bubbling with nitrogen gas in a flotation cell. Metal ions in MIBK solution were measured by graphite furnace-AAS. Experimental conditions were optimized as follow so. After the pH of a 1.0 L water sample was adjusted to 5.0, 6.0 mL of 0.1 M 1-HNph and 10 mL of 0.03 M TBA-bromide were added to the sample to form ion-pairs, and 2.0 mL of 0.2%(w/v) SLS was added to make the ion-pairs hydrophobic. The solution was bubbled with 30 mL/min N2 gas for 5 minutes in a flotation cell. Linear calibration curves were obtained for the determination of Zn(Ⅱ) and Pb(Ⅱ) in several water samples. Reproducible results of showing a relative standard deviation of < 10% and recoveries of 80-100% could be obtained.

• Journal of Pharmaceutical Investigation
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• v.4 no.1_2
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• pp.46-54
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• 1974

A new spectrophotemetric method was estalished for the determination of oleic acid. This method is based on the 1,2-dichloroe-thane extraction of the ion-pair formed between methylene blue and oleic acid. But the absorbance of an ion-pair in the 1,2-dichloroe-thane layer was variable with the temperature, the ion-pair was extracted back into a diluted hydrochloric acid solution. The maximum absorbance of the acid extract observed at $660m{\mu}$ and a lineal relationship was observed from the initial amount over the range of $50-800{\gamma}/ml$ of oleic acid in the aqueous phase. The composition ratio of the ion-pair formed between methylene blue and oleic acid was determined to be 2 : 1 by both the mole ratio and continuous variation methods.

• YAKHAK HOEJI
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• v.35 no.1
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• pp.15-21
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• 1991

Quaternary amines which are widely used as medicines are nitrogen compounds. Metanil yellow(MY) and benzalkonium chloride(BKC) were mixed and added to 10ml of the buffer solution and then the solution was shaken for 5 minutes. The maximum absorption wavelength of the reaction product was 402 nm. Dichloromethane was the best extracting solvent among the several organic solvents and the most suitable pH range was 2~8. When the BKC-MY calibration curve was made in the best experimental condition, the Lambert-Beer's law was obeyed in the range of BKC concentration of 2$\times$$10^{-6}$~9$\times$$10^{-6}$M by UV spectrophotometer. This method was possible to determine quaternary ammonium salts in the pharmaceutical preparation.