• 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%.

• Bulletin of the Korean Chemical Society
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• v.22 no.1
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• pp.19-24
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• 2001

A solvent sublation has been studied for the determination of trace Au(III), Pt(IV) and Pd(II) in waste water with their complexes of 2-mercaptobenzothiazole (MBT). Experimental conditions such as the concentration of HCl, the amount of MBT as a ligand, the type and amount of surfactants, bubbling rate and time, and the type of organic solvent were optimized for the solvent sublation, i.e., 25.0 mL of 2.0 M HCl solution and 30mL of 0.4%(w/v) MBT ethanolic solution were added to a 1.0 L sample to form stable complexes. The addition of 4.0 mL of 1 ${\times}$$10^{-3}$ M CTAB (cetyltrimehtylammonium bromide) solution was needed for the effective flotation accomplished by bubbling nitrogen gas at the rate of 40.0 mL/min for 35 minutes. As a solvent, 20.0 mL of MIBK (methylisobuthylketone) was used to extract the floated complexes. The procedure was applied to three kinds of waste waters. Au(III) was determined as 0.68 ng/mL and 0.98 ng/mL respectively for final washed water of two plating industries in Banwol. Pd(II) and Pt(IV) were not detected in any of the three samples. The recovery, which was obtained with analyte-spiked samples, were 95-120%.

• Bulletin of the Korean Chemical Society
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• v.27 no.11
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• pp.1757-1762
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• 2006

A solvent sublation using salphen as a ligand was studied and applied for the determination of trace Ni(II), Co(II) and Cu(II) in water samples. The fundamental study was investigated by a solvent extraction process because the solvent sublation was done by extracting the floated analytes into an organic solvent from the aqueous solution. The salphen complexes of Ni(II), Co(II) and Cu(II) ions were formed in an alkaline solution of more than pH 8 and then they were extracted into m-xylene. It was known that the each metallic ion formed 1 : 1 complex with the salphen and the logarithmic values of extraction constants for the complexes were 3.3 5.1 as an average value. Based on the preliminary study, the procedure was fixed for the separation and concentration of the analytes in samples. Various conditions such as the pH of solutions, the influence of $NaClO_4$, the bubbling rate and time of $N_2$ gas, and the type of organic solvent were optimized. The metal-salphen complexes could be extracted into m-xylene from the solution of more than pH 8, but the pH could be shifted to acidic solution of pH 6 by the addition of $NaClO_4$. In addition, the solvent sublation efficiency of the analytes was increased by adding $NaClO_4$. The recovery of 97-115% was obtained in the spiked samples in which given amounts of 0.3 mg/L Ni(II), 0.8 mg/L Co(II) and 0.04 mg/L Cu(II) were added.

• Analytical Science and Technology
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• v.16 no.4
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• pp.1029-1040
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• 2003

• Bulletin of the Korean Chemical Society
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• v.19 no.10
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• pp.1036-1042
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• 1998

The preconcentration and determination of trace elements in water samples were studied by a solvent sublation utilizing dithizonate complexation. After metal dithizonates were formed, trace amounts of cadmium, cobalt, copper and lead were floated and extracted into small volume of a water-immiscible organic solvent on the surface of sample solution and determined in the solvent directly by GF-AAS. Several experimental conditions as formation condition of metal-dithizonate complexes, pH of solution, amount of dithizone, stirring time, the type and amount of surfactants, N2 bubbling rate and so on were optimized for the complete formation and effective flotation of the complexes. And also four kinds of light solvents were compared each other to extract the floated complexes, effectively. After the pH was adjusted to 4.0 with 5 M HNO3, 8.0 mL of 0.05% acetone solution of dithizone was added to 1.00 L water sample. The dithizonate complexes were flotated and extracted into the upper methyl isobutylketone (MIBK) layer by the addition of 2.0 mL 0.2% ethanolic sodium lauryl sulfate solution and with the aid of small nitrogen gas bubbles. And this solvent sublation method was applied to the analysis of real water samples and good results of more than 85% recoveries were obtained in spiked samples.

• Bulletin of the Korean Chemical Society
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• v.19 no.1
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• pp.50-56
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• 1998

A solvent sublation was studied for the determination of trace Cd, Co, Cu and Ni in water samples. Ammonium pyrrolidine dithiocarbamate (APDC) was used as a complexing agent. Experimental conditions such as pH of solution, amounts of APDC, the type and amount of surfactant, the type of solvent, etc. were optimized for the effective sublation of analytes. After metal-PDC complexes were formed in sample solutions of pH 2.5, the precipitate-type complexes were floated in a flotation cell with an aid of sodium lauryl sulfate as a surfactant and by bubbling with nitrogen gas. The precipitates were dissolved and separated into the surface layer of methyl iso-butyl ketone (MIBK). The analytes preconcentrated were determined by a graphite furnace atomic absorption spectrophotometry (GF-AAS). Extractability of each element was 88% for Cd(Ⅱ), 86% for Co(Ⅱ), 95% for Cu(Ⅱ) and 76% for Ni(Ⅱ), respectively. And this procedure was applied to the analysis of real samples. From the recoveries of more than 92%, it was concluded that this method could be simple and applicable for the determination of trace elements in various water samples of a large volume.

• 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.

• Bulletin of the Korean Chemical Society
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• v.24 no.12
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• pp.1775-1780
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• 2003

A continuous flow system has been developed to determine trace Cu(II), Mn(II), Ni(II) and Zn(II) in a large volume of water samples by a solvent sublation technique. The mixed solution of 1,10-phenanthroline(phen) and thiocyanate ion was used as ligands for the formation of their ternary complexes. The continuous system was constructed in this laboratory with a peristaltic pump, a mini shaker, three mixing bottles and a flotation cell by connecting each part with a polyethylene tube. The flotation conditions such as the flow rate of sample solution and the injection rates of ligand, buffer and surfactant solutions have been investigated to obtain the best sublation efficiencies. Each solution flowed into the flotation cell through each polyethylene tube by the peristaltic pumps. The ternary complexes were floated and extracted into MIBK in a flotation cell of 2 L by bubbling a nitrogen gas. The absorbances of extracted analytes in MIBK were directly measured by graphite furnace-AAS. The concentrations of 1,10-phenanthroline and thiocyanate ion were $2.6\;{\times}\;10^{-3}$ M and $2.3\;{\times}\;10^{-2}$ M in the mixed solution, respectively. The pH of sample solution was adjusted to 5.0 with a buffer solution and 1%(m/v) sodium lauryl sulphate solution was added as a surfactant to support the effective flotation of the complexes. The $N_2$ gas was bubbled at 30 mL/min for 90 minutes for 20 L of sample. Reproducible results of less than 10% RSD and recoveries of 80-120% could be obtained in real samples.

• Nuclear Engineering and Technology
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• v.15 no.2
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• pp.149-153
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• 1983

The removal of zinc (II) from aqueous solutions has been studied by the adsorptive bubble separation processes such as solvent sublation and foam fractionation processes using capric acid as collector. The efficiency of the remoal process has been studied by changing the ionic strength and pH and the bubble separation method has been compared with the solvent extraction process using the capric acid dissolved in benzene as extractant.