• Bulletin of the Korean Chemical Society
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• v.20 no.4
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• pp.431-435
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• 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.

• 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.

• Journal of the Korean Chemical Society
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• v.54 no.3
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• pp.283-286
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• 2010

A sensitive and reproducible method for the flotation-spectrophotometric determination of zirconium is reported. The method is based on the complex formation zirconium and xylenol orange (XO) which is floated in the interface of aqueous phase and n-hexane by vigorous shaking. By discarding the aqueous solution and n-hexane, the adsorbed complex on to the wall of a separating funnel was dissolved in a small volume of methanol solvent and its absorbance was measured at 429 nm. The effect of different parameters such as pH, concentrations of HCl, and XO, and volume of n-hexane flotation dissolvent, standing and shaking time were studied. The calibration curve was linear in the range of 7-120 ng $mL^{-1}$ of zirconium with a correlation coefficient of 0.9991. The limit of detection (LOD) was 5.8 ng $mL^{-1}$. The relative standard deviation (RSD) for seven replicate measurements of 50 and 110 ng $mL^{-1}$ of zirconium were 4.4 and 3.0%, respectively. The method was successfully applied to the determination of zirconium in water samples.

• Bulletin of the Korean Chemical Society
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• v.26 no.10
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• pp.1529-1532
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• 2005

A simple and cost effective method for separation and preconcentration of Ag(I) at the $10^{-7}\;mol\;L^{-1}$ level in the environmental and mineral samples is present. The method is based on the flotation of Ag(I)-iodide complex as an ion-associate with ferroin in pH of 4 from a large volume of an aqueous solution (500 mL) using nheptane. The floated layer was then dissolved in dimethylsulfoxide (DMSO) for the subsequent spectrophotometric determination. Beer's law was obeyed over a range of 2.0 ${\times}$ $10^{-7}$-4.0 ${\times}$ $10^{-6}$ mol $L^{-1}$ with the apparent molar absorptivity of 2.67 ${\times}$ $10^5$ L $mol^{-1}\;cm^{-1}$. The detection limit (n = 5) was 4 ${\times}$ $10^{-8}$ mol $L^{-1}$, and RSD (n = 5) obtained for 2.0 ${\times}$ $10^{-6}$ mol $L^{-1}$ of Ag(I) was 2.2%. The interference effects of a number of elements was studied and found that only $Hg^{2+}$ at low concentration, and $Pb^{2+}$, $Cd^{2+}$, $Cu^{2+}$, and $Fe^{3+}$ ions at moderately high concentrations were interfered. To overcome on these interference effects, the solution was treated with EDTA at a buffering pH of 4 and passed through a column containing Amberlite IR-120 ionexchanger resin, just before the flotation process. The proposed method was applied to determine of Ag(I) in a synthetic waste water, a photographic washing sample and a geological sample and the results was compared with those obtained from the flame atomic absorption spectrometry. The results were satisfactorily comparable with together, so that the applicability of the proposed method was confirmed in encountering with the real samples.

• Journal of the Korean Chemical Society
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• v.40 no.12
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• pp.724-732
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• 1996

The organic precipitate flotation using Cu(II)-pyrrolidinedithiocarbamate complex as a coprecipitant was studied for the preconcentration and determination of trace Cd, Pb, Bi and Co in several water samples. Experimental conditions such as pH of solution, amounts of Cu(II) and ammonium pyrrolidinedithiocarbamate(APDC), stirring time, the type and amount of surfactant, etc. were optimized for the effective flotation of analytes. After 3.0 mL of 1,000 ${\mu}g/mL$ Cu(II) solution was added to 1.00 L water sample, the pH of the solution was adjusted to 2.5 with HNO3 solution. Trace amounts of analytes were coprecipitated by adding 2.0% APDC solution. And the precipitates were flotated onto the surface of solution with the aid of nitrogen gas and sodium lauryl sulfate. The floats were collected from mother liquor, and filtered through the micropore glass filter by suction. The precipitates were dissolved with 4 mL conc. HNO3, and then diluted to 25.00 mL with deionized water. The analytes were determined by graphite furnace atomic absorption spectrophotometry. This flotation technique was applied to the analysis of some water samples, and the 90 to 120% of recoveries were obtained from the spiked samples, this procedure could be concluded to be simple and applicable for the trace element analysis in various kinds of water.

• Analytical Science and Technology
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• v.5 no.4
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• pp.425-431
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• 1992

The concentration and determination of trace phosphate ion was studied by $La(OH)_3$ coprecipitaiton. Phosphate ions in 1.0L samples were coprecipitated with lanthanium hydroxide at pH 9.5 adjusted with ammonia solution. The precipitates were floated with the aid of mixed surfactant(1:8 sodium oleate/sodium dodecyl sulfate) and nitrogen gas bubbles. The floated precipitate was collected in suction flask from the solution. The precipitate were washed with dil. ammonia solution and dissolved in sulfuric acid. The phosphate ion in the concentrated solution was finally determinated by UV/VIS spectrophotometry using the molybdenium blue method. The proposed method could be applied to the determination of phosphate ion in tap water and river water.

• Journal of the Korean Chemical Society
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• v.38 no.9
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• pp.667-675
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• 1994

The precipitate flotation using $La(OH)_3$ as a coprecipitant was studied for the simultaneous determination of trace three elements in a sea water. Several experimental conditions such as pH, coprecipitant and surfactant were investigated with an artificial sea water. To remove the influence of Cr(VI) the Cr(VI) was reduced to Cr(III) using $NaBH_4$ prior to the flotation. Trace amounts of Cu(II), Co(II) and total Cr in 1.0 l sea water was coprecipitated together with the precipitation of $La(OH)_3$ in the solution of pH 9.8 adjusted with 3.OM NaOH solution. The precipitate was floated by using a mixed surfactant (1 to 8 of each 0.5% ethanolic sodium oleate and sodium dodecylsulfate solution) by bubbling a nitrogen gas. The floats was separated and filtrated from the mother liquor by suction. The precipitate was dissolved in 7.0 M $HNO_3$ solution and then marked to 25.0 ml with a deionized water. These elements were determined by graphite fumace atomic absorption spectrophotometry. This method was applied to determine the elements in the sea water of the Eastern and Western coasts. And the recoveries were over 90.0% in the samples into which given amounts of the analyte elements were spiked.

• 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%.

• Journal of the Korean Chemical Society
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• v.35 no.4
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• pp.355-361
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• 1991

The separative preconcentration of trace mercury[Hg(II)] in a water sample was studied by a coprecipitation flotation technique. The trace Hg(II) was precipitated together with Ce(OH)$_3$ by adding 3.0 ml of 0.1M Ce$^{3+}$ solution to 1,000 ml of water sample and adjusting pH to 11.0 with 1.0M NaOH solution. The hydrophobic precipitate[Ce(OH)$_3$-Hg(OH)$_2$], which was formed by adding 2.0 ml of 0.1${\%}$ ethanolic sodium oleate solution, were floated on the surface with an aid of tiny nitrogen gas bubbles. The floated materials were quatitatively collected in a suction flask and dissolved with 5.0 ml of 2.0M HNO$_3$. The solution was marked to 25.00 ml with a deionized water. The content of Hg(II) was determined by cold vapor atomic absorption spectrophotometry. Any interferences of concomitants such as Ag$^+$, Br$^-$, I$^- $, etc. were not observed on the whole procedure. The analytical result showed that Hg(II) found in the wastewater of Seochang Campus, Korea University was 1.98 ng/ml with the relative standard deviation of 3.6${\%}$. And recoveries of Hg(II) in the wastewater into which 1.0 ng/ml and 2.0 ng/ml were added were 95${\%}$ and 91${\%}$, respectively. From such results, this procedure could be concluded to be tolerably accurate and reproducible for the determination of trace mercury in a water sample.