• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.4 no.2
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• pp.189-197
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• 1994

Analytic methods for Cr(VI) level in industrial hygienic field were suggested by the National Institute for Occupational Safety and Health(NIOSH method 7600, 7604). There were growing needs for measurement of Cr(III) and Cr(VI) levels simultaneously. Two analytical methods were suggested to determine Cr(III) and Cr(VI) levels simultaneously. The one is method by using reversed phase high peformance liquid chromatography(HPLC) and the other is by using ion exchange HPLC. The purpose of this work was to evaluate the usefulness of these two analytic methods. For the difference of ionic charges of Cr(III)-ethylendiamine tetraacetic acid(EDTA) chelate and $CrO_4{^-2}$, we could detect them simultaneously by ion exchange HPLC. Also, we attempted to determine the levels of Cr(III) and Cr(VI) chelated with sodium diethyldithiocarbamate(NaDDTC) by using reversed phase HPLC. The confirmation of Cr(III) and Cr(VI) were checked by fraction collector and nameless atomic absorption spectrometer. The optimal conditions for the formation of Cr(III)-EDTA chelate were two hours incubation period with pH 5. Cr(III)-EDTA and Cr(VI) in EDTA solution were successfully separated by anion exchange column using $Na_2CO_3/NaOH$ mixture as mobile phase. Peaks of Cr(III)-EDTA and Cr(VI) in EDTA were identified at 5 minutes and 7 minutes of retention time respectively by the ion exchange HPLC. The formation of Cr(III)-NaDDTC and Cr(VI)-NaDDTC chelates were twelve hours incubation period. Cr(III)-NaDDTC and Cr(VI)-NaDDTC chelates were separated by reversed phase column using methanol and water mixture as mobile phase. Peaks of Cr(VI)NaDDTC and Cr(III)-NaDDTC chelates were identified at 13 minutes and 26 minutes of retention time respectively by the reversed phase HPLC. Due to reduction of Cr(VI) to Cr(III), it seems to be not suitable for simultaneous determination of Cr(III)-NaDDTC and Cr(VI)-NaDDTC chelates by reversed phase HPLS. Simultaneos determination of Cr(III) and Cr(VI) by ion exchange HPLC was more accurate and simple method.

• Bulletin of the Korean Chemical Society
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• v.27 no.5
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• pp.694-698
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• 2006

A method has been described for the chemical speciation, preconcentration and determination of Cr(III) and Cr(VI) species in filtered tannery waste waters by flame atomic absorption spectrometry using ion-exchange resins. Amberlite IR-120($H^+$) strongly acidic cation exchanger and Amberlite IRA-410($CI ^-$) strongly basic anion exchanger resins were used for the separation and preconcentration of Cr(III) and Cr(VI) species, respectively. Optimum condition for preconcentration and speciation was obtained by testing pH of sample and eluent, flow rates of sample and eluent, amount of resins, volume of sample and eluents, and effect of foreign ions. The recommended method has been successfully applied for the preconcentration and determination of chromium species in the dissolved phase of waste water samples collected from a tannery waste water treatment plant in Kayseri, Turkey. The detection limits achieved were 0.73 $\mu$g/L for Cr(III) and 0.81 $\mu$g/L for Cr(VI). Recovery studies showed 99% for Cr(III) and 98% for Cr(VI), for samples spiked with single species.

• Analytical Science and Technology
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• v.17 no.3
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• pp.199-210
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• 2004

A new polystyrene-divinylbenzene chelating resin containing 4,5-dihydroxy-naphthalene-2,7-disulfonic acid (chromotropic acid : CTA) as functional group has been synthesized and characterized. The sorption and desorption properties of this chelating resin for Cr(III) ion and Cr(VI) ion including nine metal bloodstain. As a results, FOB test kit could be effectively applied to identification of human blood at chelating resin was stable in acidic and alkaline solution. The Cr(VI) ion is selectively separated from Cr (III) ion at pH 2 and the maximum sorption capacity of Cr(VI) ion is 1.2 mmol/g. In the presence of anions such as $F^-$, $SO{_4}^{2-}$, $CN^-$, $CH_3COO^-$, $NO{_3}^-$, the sorption of Cr(VI) ion was reduced but anions such as $PO{_4}^{3-}$ and $Cl^-$ revealed no interference effect. The elution order of metal ions obtained from breakthrough capacity and overall capacity at pH 2 was Cr(VI)>Sn(II)>Fe(III)>Cu(II)>Cd(II)${\simeq}Pb(II){\simeq}Cr(III){\simeq}Mn(II){\simeq}Ni(II){\simeq}Al(III)$. Desorption characteristics for Cr(VI) ion was investigated with desorption agents such as $HNO_3$, HCl, and $H_2SO_4$. It was found that the ion showed high desorption efficiency with 3 M HCl. As the result, the chelating resin, XAD-16-CTA was successfully applied to separation and preconcentration of Cr (VI) ion from several metal ions in metal finishing works.

• Advances in environmental research
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• v.1 no.2
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• pp.167-179
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• 2012

Pistachio shell (Pistacia vera) (PS), a low-cost material, has been utilized for the removal of the Cr(VI) ions after treatment with citric acid. Batch experimental steps were applied to obtain Cr(VI) ion adsorption details for the equilibrium between Cr(VI) and modified pistachio shell (MPS). The influences of contact time, pH, adsorbent dose and initial chromium concentration on the adsorption performance of MPS was investigated in detail. The results displayed that adsorption of Cr(VI) by MPS reached to equilibrium after 2 h and after that a little change of Cr(VI) removal efficiency was observed. The sorption percent is higher at lower pH and lower chromium concentration. Two possible mechanisms for reduction of Cr(VI) to Cr(III) can be suggested in Cr(VI) removal. In the first mechanism, Cr(VI) is reduced to Cr(III) by surface electron-donor groups of the adsorbent and the reduced Cr(III) forms complexes with adsorbent or remains in the solution. This Cr(III) is not adsorbed by adsorbent at pH 1.8. But in second mechanism, the adsorption-coupled reduction of Cr(VI) to Cr(III) occurred on the adsorbent sites. The equilibrium sorption capacity of Cr(VI) ion after 2 h was 64.35 mg/g for MPS.

• Journal of the Korean Chemical Society
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• v.46 no.2
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• pp.145-150
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• 2002

A Method to determine Cr(III)ion in aqueous solution by chemiluminescence method using a stopped flow system has been studied. The method is based on the increased chemiluminescence intensity with the addition of Cr(III) to a solution of lucigenin a nd hyrogen peroxide. The effects of pH, injection volumes of reagent and sample, and concentration of lucigenin and hyrogen peroxide on the chemiluminescence intensity have been investigated. The calibration curve for Cr(III) ion was linear over the range from 1.0${\times}$$10^{-6}$ to 1.0${\times}$$10^{-3}$M and the detection limit was 5.2${\times}$$10^{-8}$M under the optimal experimental condition of 437nm, 12.8,and 1.0${\times}$$10^{-6}$ and 2.0M for emission wavelength, pH, and concentration of lucigenin and hyrogen peroxide, respectively.

• Polymer(Korea)
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• v.25 no.6
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• pp.765-773
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• 2001

In In order to remove harmful trace elements such as $Co^{2+}$, $Ni^{2+}$ , $Cr_2O_7\;^{2-}$ from water, we synthesized AN-co-(MMA/IA) according to various mole ratio of monomers and spun by wet-spinning. And multi-functional PAN ion exchangers were prepared by hydrolysis. We observed structure, degree of functionalization, ion exchange capacity, distribution coefficient and mechanical properties for ion exchanger. Anion exchange capacity decreased in 4.5 ~ 4.2 meq/g with increasing of IA content and cation exchange capacity increased in 1.8 ~ 2.2 meq/g. Tensile strength of the ion exchanger increased up to 0.008 mol% IA content and appeared maximum value by 216$kg/cm^2$Distribution coefficient for AN-co-(MMA/IA) ion exchanger appeared maximum value for Co(II), Ni(II) in pH 5-6 range and for Cr(III) in pH 3-4 range. And the adsorption capacity was in the order of Cr(III) > Co(II) > Ni(II) for multicomponent in continuous process.

• Journal of the Korean Chemical Society
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• v.25 no.4
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• pp.270-274
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• 1981

Al(III) and Cr(III) were determined selectively by colorimetry of Bismark Brown R {4,4'[(4-methyl-1,3-phenylene)bis(azo)]-bis(6-methyl-1,3-benzenediamine) dihydrochloride} in the presence of the various cations and anions without the using of any masking agents, but tartrate and citrate ions were interfered. The ligand of Bismark Brown R and complexes of Al(III) and Cr(III) were shown the maximum absorbance at the same wavelength together and both metallic ion were interfered to determine each other, but Al(III) were able to determine after oxidation of Cr(III) to Cr(VI).

• Bulletin of the Korean Chemical Society
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• v.27 no.5
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• pp.687-693
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• 2006

Chromium(III) complexes, cis-[Cr([14]-decane)$(HOC _6H _4COO) _2$]$ClO _4$ I and cis-[Cr([14]-decane)(OH) $(OC _6H _4NO _2)$]$ClO _4{\cdot}H _2O$ II ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) are synthesized and structurally characterized by a combination of elemental analysis, conductivity, IR and VIS spectroscopy, and X-ray crystallography. The complexes crystallizes in the monoclinic space groups, $C2 _1$/a in I and $P2 _1$/n in II. Analysis of the crystal structure of complex I reveals that central chromium(III) ion has a distorted octahedral coordination environment and two hydrogensalicylato ligands are unidentate to the chromium(III) ion via the carboxyl groups in the cis-position. For monomeric complex I the hydrogensalicylato coordination geometry is as follows: Cr-O(average) = 1.984(3) $\AA$;Cr-N range = 2.105(3)-2.141(4) $\AA$;C(24)-O(4) = 1.286(5) $\AA$;N(2)-Cr-N(4) (equatorial position) = 96.97(15)${^{\circ}}$; N(1)-Cr-N(3) (axial position) = 168.27(15)${^{\circ}}$; O(1)-Cr-O(4) = 85.70(13)${^{\circ}}$. The crystal structure of II has indicated that chromium(III) ion is six-coordinated by four secondary amines of the macrocycle, hydroxide anion and nitrophenolate anion.

• Bulletin of the Korean Chemical Society
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• v.26 no.7
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• pp.1044-1050
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• 2005

The reaction of cis-[Cr([14]-decane)($OH_2)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = isothiocyanate ($NCS^-$), azide ($N3^-$) or chloroacetate(caa)} leads to a new cis-[Cr([14]-decane)($NCS)_2]ClO_4{\cdot}H_2O$ (1), cis-[Cr([14]-decane)($N_3)_2]ClO_4$ (2) or cis-[Cr([14]-decane)($caa)_2]ClO_4$ (3). These complexes have been characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[Cr([14]-decane)($NCS)_2]ClO_4{\cdot}H_2O$ reveals that central chromium(III) has a distorted octahedral coordination environment and two $NCS^-$anions are bonded to the chromium(III) ion via the Ndonor atom in the cis positions. The angle $N_{axial}-Cr-N_{axial}$ deviates by 13$^{\circ}$ from the ideal value of 180$^{\circ}$ for a perfect octahedron. The bond angle N-Cr-N between the Cr(III) ion and the two nitrogen atoms of the isothiocyanate ligands is close to 90$^{\circ}$. The bond lengths of Cr-N between the chromium and $NCS^-$groups are 1.964(5) and 2.000(5) $\AA$. They are shorter than those between chromium and nitrogen atoms of the macrocycle. The IR spectra of 1, 2 and 3 display bands at 2073, 1344 and 1684 $cm^{-1}$ attributed to the $NCS^-$, ${N_3}^-$ and caa groups stretching vibrations, respectively.

• Journal of the Korean Chemical Society
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• v.30 no.5
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• pp.423-432
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• 1986

Atomic absorption spectrophotometric (AAS) determination of hexavalent chromium [Cr(VI)] in a waste water was studied. Cr(VI) was extracted with p-xylene from the wastewater, in the way of ion pair formation with anion exchanger aliquat-336(tri-caprylmethyl ammonium chloride). 100ml waste water, after organic materials were extracted out with toluene, was acidified with conc. HCl adjusting the medium to pH 0.5 and 20ml of p-xylene containing 0.01M aliguat-336 was used to extract Cr(VI) from the acidified solution. The absorbance of chromium was measured with air-acetylene flame at 357.9nm. Standard addition method was used in the determining concentration of Cr(VI) extracted. No interference has been found in the extraction of Cr(VI) by the Al(III), Fe(III) and Cr(III) ion presented. However, Fe(II) decreased the absorbance of Cr(VI), due to the fact Fe(II) reduces Cr(VI) to Cr(III). The contained organic material was removed prior to extracting process, since it may reduced the absorbance of Cr(VI). The recovery of added Cr(VI) was over 96%, which seems to be promising and the relative standard deviation was 3.95%