Matrix separation of palladium and iridium by the cellulose anion exchanger Cellex T and the subsequent determination of palladium at theμg/g-level

The preconcentration and separation of palladium and iridium from base metals is studied with cellulose (Cellex T) and styrene-divinylbenzene (Varion AT 400) anion exchangers. In spite of lower capacity of Cellex T to chloride complexes of Pd and Ir, it allowed to get a higher preconcentration factor. Yields of 92–99% are achieved for Pd and 96–97% for Ir from the solutions containing great excess of base and heavy metals. Graphite furnace atomic absorption spectrometry is used for the final measurements. The procedure has been applied to the determination of palladium in natural samples.     

Multielement Preconcentration and Removal of Trace Metals by Solid-Phase Extraction

ABSTRACT

The solid phase extraction of trace amounts of some metal ions from their mixtures using cation exchanger Dowex 50Wx4, cellulose sorbent with phosphonic acid groups Cellex P, chelating resin Chelex 100 and SIO₂-TPP sorbent which contains porphyrin ligand covalently attached to aminopropyl silica gel was investigated. With respect to multielement preconcentration Cellex P and Chelex 100 seem to be the best sorbents; the recovery test for Al, Be, Cd, Ni, Pb and Zn were > 90%. Additionally, Cellex P appeared to be suitable for enrichment of Co and Mn. Silica-TPP sorbent could be applied as a selective collector for Mo(VI) and V(IV).     

Chromatographic behaviour of alkaloids on thin layers of anion and cation exhangers. I. AG 1-X4 and cellex D.

The chromatographic behaviour of 48 alkaloids has been studied on Bio-Rad AG 1-X4, Cellex D and microcrystalline cellulose, eluting with solutions of different pH but constant ionic strength (0.5). Many interesting separations were effected on both AG 1-X4 and Cellex D layers. The influence of pH on the chromatographic behaviour of alkaloids has been quantitatively studied and an equation was used that expresses the behaviour of the alkaloids on both AG 1-X4 (AcO-) and microcrystalling cellulose layers. The nonapplicability of this equation to Cellex D layers is discussed.     

Application of the ion-exchanger Cellex P for the selective separation of some metal ions

Summary The selectivity of the cellulose ion-exchanger Cellex P containing phosphonic groups has been examined by means of tetrene. The affinity of 14 metal ions was determined as a function of the pH-value in the presence of tetrene. Bismuth was separated from large excess of Pb, Cd, Cu, Co, Ni, Fe, Mn and Zn by means of this ion-exchanger using tetrene as a complexing agent. The method has been applied to the determination of bismuth in metallic lead.

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Anwendung des Ionenaustauschers Cellex P zur selektiven Abtrennung einiger MetallionenTeil 3. Quantitative Abtrennung des Bismuts von anderen Elementen in Gegenwart von Tetraethylenpentamin (Tetren) als Komplexierungsmittel

Zusammenfassung Die Selektivität des Phosphonsäuregruppen-haltigen Celluloseaustauschers Cellex P wurde mit Hilfe von Tetren untersucht. Die Affinität von 14 Metallionen wurde als Funktion des pH-Wertes in Gegenwart von Tetren bestimmt. Bismut konnte von einem großen Überschuß an Pb, Cd, Cu, Co, Ni, Fe, Mn und Zn abgetrennt werden. Das Verfahren wurde zur Bismutbestimmung in Bleimetall angewendet.

     

Gold Trace Separation from some Platinum Group Metals on Cationic Exchanger in the Presence of Amines

Abstract

The sorption behaviour of gold in the presence of amines on different kinds of cationic exchangers with phosphonic groups has bee investigated. The system Cellex P - amine has been found very useful for gold separation from platinum metals. The method was adopted for trace gold determination in PdC1₂ and platinum powder.     

Solid-Phase Extraction of Trace Amounts of Selenomethionine

Abstract

Preconcentration and separation of trace amounts of selenomethionine was investigated using several solid sorbents. The best results were obtained with copper-treated Chelex 100 chelating resin. Selenomethionine from 100 ml of solution adsorbed on 0.2 g of the resin was eluted with 8 ml of 1.5 mol/l ammonia solution and determined by electrothermal atomic absorption spectrometry. The column chromatography with Cu-Chelex and functionalized cellulose sorbent Cellex T was applied to separate organic and inorganic selenium forms.     

High-performance liquid chromatographic determination of free and total polyamines in human serum as fluorescamine derivatives

A highly sensitive and simple fluorimetric method for the determination of free and total polyamines, spermidine, spermine, putrescine and cadaverine, in human serum by high-performance liquid chromatography is described. The polyamines, obtained after clean-up of deproteinized serum by Cellex P column chromatography, are converted to their fluorescamine derivatives in the presence of nickel ion which inhibits the reaction of interfering amines with fluorescamine, and the derivatives are separated simultaneously by reversed-phase chromatography (LiChrosorb RP-18) with a linear gradient elution. The lower limits of detection are 10 and 15 pmole for spermine and the others in 0.5 ml of serum, respectively.     

Effect of transition metals on recovery from plasma of the growth-modulating tripeptide glycylhistidyllysine

Isolation and purification of growth-modulating peptides from biological sources is often accompanied by excessive losses of bioactive material. During the isolation of a growth-modulating tripeptide glycylhistidyllysine (GHL) from human plasma, copper and iron were found to co-isolate with the peptide. Studies with [3H]GHL demonstrated that these metals interfere at several steps of the procedure for the isolation of GHL from plasma (gel filtration chromatography, high-pressure silica-gel). Removal of these metals with an insoluble chelating resin (Cellex 100) enhanced recovery of [3H]GHL from plasma 8-fold. These results suggest that removal of transition metals may aid in the recovery of peptides which are difficult to isolate from biological sources.     

Investigation of the usefulness of NTA, EDTA and DTPA in separation of some platinum metals on cellulose exchangers

The possibility of using NTA, EDTA and DTPA as complexing agents for separation of some platinum group ions on cellulose ion-exchangers has been investigated. The greatest differences in the affinities of Pd(II) and Pt(IV) toward the cellulose ion-exchangers are obtained in the presence of DPTA, Cellex D (as ion-exchanger) in hydroxide form. The column separation of Pd(II) from Pt(IV), Rh(III) from Pd(II) and of a Rh(III)Pd(II)Pt(IV) mixture can be achieved with DPTA and chloride solutions. The method can be for determination of the components of RhPdPt alloys.     

CHARACTERIZATION OF CIS- AND TRANS-DINITROBIS-(l-CYCLOHEXANEDIAMINE)-COBALT(III) CHLORIDE1

Abstract

Two geometrical isomers of [Co(l-chxn)₂(No₂)₂]Cl have been isolated. The trans-isomer is eluted first from a cellulose ion exchange column as a single isomer. The cis-isomer corresponds to the complex previously reported as the trans-isomer. The cis-isomer with the same CD sign pattern as for the trans-isomer is stereoselectively favored, but a small amount of the second cis-isomer separates using Cellex CM ion exchange cellulose. The CD spectra of the cis- and trans- isomers are similar to those of the corresponding isomers of the l-pn complex.     

Flame AAS determination of lead in water with flow-injection preconcentration and speciation using functionalized cellulose sorbent

The on-line solid phase extraction of trace amount of lead in flow-injection system with flame AAS detection was investigated using cellulose sorbents with phosphonic acid and carboxymethyl groups, C(18) sorbent non-modified and modified with Pyrocatechol Violet or 8-quinolinol, commercial chelating sorbents Chelex 100 and Spheron Oxin 1000, non-polar sorbent Amberlite XAD-2 modified with Pyrocatechol Violet and several cation-exchange resins. The best dynamic characteristics of retention were observed for functionalized cellulose sorbents. For Cellex P assumed as optimum sorbent, elution with a separate fractions of nitric acid and ethanol allows the differentiation between tetraalkyllead and sum of inorganic lead and organolead species of smaller number of alkyl groups. The detection limit for the determination of inorganic Pb(II) was estimated as 0.17 microg/l. at preconcentration from 50 ml sample at a flow rate of 7 ml/min.     

The application of solid sorbents for the purification of aluminum contaminated chemicals used as modifiers in electrothermal atomic absorption spectrometry

Various microcolumns with solid sorbents (ion exchange resins, functionalised cellulose sorbents, chelating resins) have been tested with respect to their ability for the purification of aluminum contaminated chemicals used as modifiers in electrothermal atomic absorption spectrometry. The purification of NaNO(3), Mg(NO(3))(2), K(2)SO(4) and (NH(4))(2)HPO(4) has been the most effective with an almost 100% efficiency, when Spheron-Oxine was used as chelating resin. The sorption of aluminum from KOH solution has been found to be very high (around 90%) for all investigated sorbents. However, the best results have been obtained with anion-exchange resins. It has been difficult to purify concentrated mineral acids (HCl, H(2)SO(4)). A retention of aluminum above 80% has been achieved only when Cellex P, Chelex 100 or Amberlite XAD-2 have been used.     

The application of solid sorbents for the purification of aluminum contaminated chemicals used as modifiers in electrothermal atomic absorption spectrometry

Various microcolumns with solid sorbents (ion exchange resins, functionalised cellulose sorbents, chelating resins) have been tested with respect to their ability for the purification of aluminum contaminated chemicals used as modifiers in electrothermal atomic absorption spectrometry. The purification of NaNO₃, Mg(NO₃)₂, K₂SO₄ and (NH₄)₂HPO₄ has been the most effective with an almost 100% efficiency, when Spheron-Oxine was used as chelating resin. The sorption of aluminum from KOH solution has been found to be very high (around 90%) for all investigated sorbents. However, the best results have been obtained with anion-exchange resins. It has been difficult to purify concentrated mineral acids (HCl, H₂SO₄). A retention of aluminum above 80% has been achieved only when Cellex P, Chelex 100 or Amberlite XAD-2 have been used.     

Variation of 7Be concentration in surface air at Nagano, Japan

The concentration of ⁷Be in surface air at Nagano City has been measured during the period from August 2000 to March 2005. The average monthly concentrations of ⁷Be in surface air were in the range of 3.3–14 mBq/m³ with pronounced two peaks in spring and autumn. It took 30–40 hours to recover the ⁷Be concentrations observed before, once ⁷Be was washed out by wet precipitations. For a pronounced increase in the concentrations of ⁷Be found in winter, a low-pressure trough coming close to the Japanese Islands with high concentrations of ⁷Be is responsible under the characteristic distribution of atmospheric pressure around the Japanese Islands.     

Stratification and tributyltin variability in San Diego Bay

Tributyltin (TBT), a biocidal antifoulant in many marine paints, was measured in near-surface and near-bottom water over a 25 h period at the entrance to a marina in San Diego Bay, USA. Surface water concentrations varied from 20 to 225 nanograms per liter (ng dm^?3) as TBT chloride and bottom water varied from non-detectable (<1 ng dm^?3) to 77 ng dm^?3. Surface water concentrations varied, with highest concentrations associated with ebbing tides, and lowest concentrations with flooding tides, indicating that the yacht basin is a source of TBT. Bottom water TBT concentrations were almost always lower than corresponding surface water concentrations. The highest bottom water concentrations were associated with flooding tides and lowest surface water TBT concentrations. Physical water column measurements indicate that vertical stratification developed during ebbing tides and dissipated during flooding tides. This accounted for maximum bottom water and minimum surface water TBT concentrations during flooding tides, due, at least in part, to vertical mixing and dilution during flood tides.     

Radioactivity in the Exclusive Economic Zone of east coast Peninsular Malaysia: distribution trends of <Superscript>137</Superscript>Cs in surface seawater

Large volumes of surface seawater samples were collected from thirty locations in the Exclusive Economic Zone (EEZ) of the east coast Peninsular Malaysia on June 2008 to study the activity concentrations of ¹³⁷Cs. The results will serve as additional information to the existing baseline data and is very useful for monitoring fresh input of anthropogenic radionuclide into Malaysian marine environment. In this study, the activity concentrations of ¹³⁷Cs were determined using co-precipitation technique, followed by Gamma Spectrometry measurement. The mean activity concentration of ¹³⁷Cs ranged between 3.40 and 5.89 Bq/m³. Higher activity concentrations were observed at the coastal and towards the south of Peninsular Malaysia and were aligned with the high turbidity. These may due to the rapid diffusion of ¹³⁷Cs from suspended particulates and fine sediments into surface seawater. The activity concentrations of ¹³⁷Cs observed in this study were slightly higher than the concentrations reported in seawater at the Straits of Malacca, Vietnam and Philippines. This might be because the study area received more input of ¹³⁷Cs that originated from global fallout and then deposited on land which later being transported subsequently into the coastal zone due to siltation and erosion processes. It could also be attributed to the intrusion of river waters containing higher concentrations of ¹³⁷Cs.     

New method for determining small concentrations of chloride ion

A new method has been devised for the determination of concentrations of chloride ion from approximately 10^-6 to 2·10^-4 M. The test solution is equilibrated with solid silver chloride, the silver ion concentration is determined by potentiometric titration with iodide ion, and the chloride concentration is calculated by the solubility product principle. Chloride concentrations near 10^-6 M can be determined with an accuracy of about ±5%, and at 10^-5 M the error is within ±0.5%. Chloride concentrations above 2-3· 10^-4 M cannot be accurately determined because of the formation of AgCl₂^-.     

Application of ion-selective electrodes in environmental analysis : Determination of Acid and Fluoride concentrations in Rain-water with a Flow-Injection System

A flow-injection method is described for the measurement of acid and fluoride concentrations. The conditions were optimized to ensure small sample and reagent consumption, low detection limit and the highest rate of analysis allowed by the potentiometric sensor. With a microcapillary pH-sensitive glass electrode, 20-μl sample volumes and 1.0–1.5 ml min^?1 carrier flow rates, strong acids were determined at concentrations as low as 10^?5 M (0.2 nmol of acid in 20 μ1). The relative standard deviation was about 1% at 10?4 M strong acid concentration at an injection rate of 500–550 h^?1. With a flow- through fluoride-selective electrode, 250-μl sample volumes and a 1 ml min^?1 carrier flow rates, fluoride concentrations as low as 10^?7 M were measured (ca. 0.5 ng of fluoride in 250 μ1). The injection rate was 40 h^?1 at concentrations below 10^?6 M, but 60 h^?1 above 10^?5 M. The methods were used successfully for determining the acid and fluoride concentrations in rain-waters.     

Temporal variations of137Cs concentrations in the surface seawater and marine organisms collected from the Japanese coast during the 1980's

The surface seawater and marine organisms were collected on the Japanese coast and analyzed for their¹³⁷Cs concentrations during the 1980's. The¹³⁷Cs concentrations in surface seawater decreased almost exponentially with time and the¹³⁷Cs removal rate constant was estimated to be 0.0445 y⁻¹. The¹³⁷Cs concentrations in marine organisms also decreased almost exponentially with time. The environmental half-lives of¹³⁷Cs in muscle and viscera of fish, crustacea, and seaweed were estimated from the measured decreases of¹³⁷Cs concentrations.