Determination of rhodium in waters by Mg-W cell-electrodeposition and electrothermal atomic absorption spectrometry

A new concentration method of rhodium using Mg-W cell-electrodeposition has been developed. The method was combined with electrothermal atomic absorption spectrometry (ETAAS) with a tungsten tube atomizer. The optimal immersing time was 120 s. The most suitable pH for rhodium electrodeposition was 1.0. Under optimal conditions, the detection limit of rhodium by the ETAAS with the preconcentration was 13 ng ml(-1) (3S/N). The severe interferences on the AAS signal of rhodium by large amounts of Ca, Cu, Fe, K, Na, Pb and Zn were eliminated by the Mg-W cell-electrodeposition method. The method was applied to the determination of rhodium in river and sea water. The recovery of rhodium spiked environmental samples was in the range of 95.6-109%. The present Mg-W cell-electrodeposition method can be utilized in in-situ sampling of trace elements in environmental samples (water). Furthermore, after sampling, it is easy to carry and store the W-sheet without contamination for a long time.     

Determination of palladium in various samples by atomic absorption spectrometry after preconcentration with dimethylglyoxime on silica gel

A preconcentration method based on the adsorption of palladium-dimethylglyoxime (DMG) complex on silica gel for the determination of palladium at trace levels by atomic absorption spectrometry (AAS) has been developed. The retained palladium as Pd(DMG)₂ complex was eluted with 1 mol l⁻¹ HCl in acetone. The effect of some analytical parameters such as pH, amount of reagent and the sample volume on the recovery of palladium was examined in synthetic solutions containing street dust matrix. The influence of some matrix ions on the recovery of palladium was investigated by using the developed method when the elements were present both individually and together. The results showed that 2500 μg ml⁻¹ Na⁺, K⁺, Mg²⁺, Al³⁺ and Fe³⁺; 5000 μg ml⁻¹ Ca²⁺ ; 500 μg ml⁻¹ Pb²⁺; 125 μg ml⁻¹ Zn²⁺; 50 μg ml⁻¹ Cu²⁺ and 25 μg ml⁻¹ Ni²⁺ did not interfere with the palladium signal. At the optimum conditions determined experimentally, the recovery for palladium was found to be 95.3±1.2% at the 95% confidence level. The relative standard deviation and limit of detection (3s/b) of the method were found to be 1.7% and 1.2 μg l⁻¹, respectively. In order to determine the adsorption behaviour of silica gel, the adsorption isotherm of palladium was studied and the binding equilibrium constant and adsorption capacity were calculated to be 0.38 l mg⁻¹ and 4.06 mg g⁻¹, respectively. The determination of palladium in various samples was performed by using both flame AAS and graphite furnace AAS. The proposed method was successfully applied for the determination of palladium in the street dust, anode slime, rock and catalytic converter samples.     

On-line determination of palladium by flame atomic absorption spectrometry coupled with a separation/preconcentration minicolumn containing a new sorbent

A method was developed for the on-line determination of palladium in complex matrices with flame atomic absorption spectrometry (FAAS) using Amberlite XAD-16 resin functionalized with 2-[2-(5-thiol-1,3,4-thiadiazolyl)]-azonaphthol (TTAN) reagent. Optimum experimental conditions such as pH of sample, type of eluent, amount of resin, volumes of sample and eluent solution, flow rates of sample and eluent, and effect of interfering ions were established. A 0.1?mol?L^?1 thiourea solution in 0.5?mol?L^?1 HCl was used as the eluent and subsequently transportation the analyte ions into the nebulizer–burner system for atomization. The synthesized chelating resin material showed excellent chemical and mechanical resistance, fast adsorption kinetics permitting the use of high sample flow rates without significant losses of retention efficiency. The detection limit of the method was 1.5?µg?L^?1 while the relative standard deviation (RSD%) was 2.4% at 0.1?mg?L^?1 Pd(II) level. The developed method was successfully applied to the determination of palladium in the catalytic converter and water samples.     

Determination of chromium by on-line preconcentration on a poly (hydroxamic acid) resin in flow-injection atomic absorption spectrometry

A series of poly(hydroxamic acid) resins were used for the preconcentration and determination of chromium(III). Conditions were optimized for the determination of chromium(III) and its separation from multi-component mixtures. A flow manifold was developed for the on-line preconcentration and determination of chromium(III) by atomic absorption spectrometry.     

Determination of platinum by atomic absorption spectrometry with chromatographic preconcentration from aqueous solutions

The conditions for determining platinum by electrothermal atomic absorption spectrometry after its extraction-chromatographic preconcentration and separation from iron(III) and copper(II) were selected. A procedure was developed that allows 0.01–0.1 mg/L platinum to be determined with a relative standard deviation of 5–7 % in the presence of 1000-fold amounts of Fe(III) and Cu(II).Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 1, 2005, pp. 41–44.Original Russian Text Copyright © 2005 by Moskvin, Yakimova, Alekseeva.     

石墨炉原子吸收法测定3-苯基丙烯酸酯类化合物中微量钯

利用高灵敏的石墨炉原子吸收法,在V(HCl):V(HNO3):V(H2O)＝5:1:94混合酸介质中测定苯基丙烯酸酯类化合物中的钯量.已纯化样品钯量的平均值是6.76 μg/g,标准相对偏差是4.8%,平均回收率为99.3%;未纯化样品钯量的平均值是121.2 μg/g,平均相对偏差是5.4%.还讨论酸介质对测定钯吸光度的影响,通过比较找到了合适的酸介质组成.     

Determination of selenium in a nickel alloy by flame atomic absorption spectrometry after electrochemical preconcentration

The nickel alloy is dissolved in nitric/hydrochloric/phosphoric acid mixture, and selenium is electrodeposited onto a platinum loop at ?0.4 V (vs. Ag/AgCl). Selenium is atomized from the electrode in an argon/hydrogen flame with simultaneous electrothermal heating of the loop. For the NBS standard nickel-based high-temperature alloy (SRM 899), the mean value found was 9.7 μg g^?1 with a standard deviation of 0.4 μg g^?1 (certified value 9.5 ± 0.1).     

Determination of palladium by flame atomic absorption spectrometry combined on-line with flow injection preconcentration using a micro-column packed with activated carbon fibre

The versatility of flow injection as a procedure for enhancing the performance of atomic spectrometry is demonstrated by the on-line separation and preconcentration of analyte ions of interest for methods employing atomic spectrometric measurements. In this paper, a sensitive method for the determination of palladium by flame atomic absorption spectrometry associated on-line with the flow injection technique has been developed. A flow system comprising a micro-column packed with activated carbon fibre was used for the concentration of palladium. In order to further enhance the performance of the analysis a new manifold with an additional column has been designed to increase the sensitivity by doubling the analytical signals. The method is sensitive and easily operating with a sampling rate of 15-20/h. The detection limit of this method is 0.3 ng/ml in standard solution and the precision is 3.9% relative standard deviation at 50 ng/ml. Recoveries of palladium in spiked solutions are 103-107%.     

Determination of selenium in biological samples by electrochemical preconcentration and atomic absorption spectrometry

Summary For the determination of selenium in biological materials the samples are digested with an HNO₃/H₂SO₄/ V₂O₅ or an HNO₃/HClO₄ mixture. Selenium is then electrolyzed onto a platinum wire, followed by atomic absorption spectrometry with simultaneous electrothermal and flame atomization. Results for the reference materials Bovine Liver and Albacore Tuna are reported (1–3±0.2 ppm Se).

---

Selenbestimmung in biologischen Proben durch elektrochemische Anreicherung und Atomabsorptionsspektrometrie

Zusammenfassung Die Proben werden mit HNO₃/H₂SO₄/V₂O₅ oder HNO₃/HClO₄ aufgeschlossen; Se wird elektrolytisch auf einem Platindraht niedergeschlagen und durch AAS mit gleichzeitiger elektrothermischer und Flammen-Atomisierung bestimmt. Ergebnisse werden mitgeteilt für die Analyse von Standardreferenzmaterialien (Bovine Liver und Albacore Tuna, 1–3±0,2 ppm Se).

     

Determination of silver in fresh water by atomic absorption spectrometry following flotation preconcentration by iron(III) collectors

Colloid precipitate flotation of silver from fresh water is applied for preconcentration and separation. Optimal conditions using hydrated iron(III) oxide and iron(III) tetramethylenedithiocarbamate as collectors were investigated. Various factors affecting the silver recovery, including collector mass, nature of the supporting electrolyte, pH of the working medium, electrokinetic potential of the collector particle surfaces, type of surfactant, induction time etc., were checked. Within the optimal pH range (5.5–6.5) silver was separated quantitatively (94.9– 100.0%) with 30 mg Fe(III) as collector. The content of silver was determined by electrothermal atomic absorption spectrometry and compared to that from inductively coupled plasma-atomic emission spectrometry. The detection limit of silver by the method described is 0.01 μg/L.     

Determination of nickel in water by electrothermal atomic absorption spectrometry with preconcentration on a tungsten foil

A preconcentration method for nickel in waters involving adsorption on tungsten foil, followed by electrothermal atomic absorption spectrometry (ETAAS) with a tungsten tube atomizer is described. The most suitable pH for nickel adsorption was 5 and the optimum immersion time was 2 min. Severe interferences from co-existing elements (Al, Ca, Cu, Fe, K, Mg, Na, Pb and Zn) on the Ni AA signal were observed. Under optimal conditions, the preconcentration of nickel on W foil could eliminate interferences from these elements. The detection limit of nickel by preconcentration-ETAAS was 0.1 ng/ml (3S/N). The method with preconcentration on tungsten foil was applied to the determination of nickel in river water. The recovery of spiked nickel was 93–102%. The tungsten foil preconcentration method is sensitive, simple, and convenient. This adsorption method can be utilized inin situ-sampling of ultra-trace nickel in environmental samples (water). Furthermore, after sampling it is easy to carry and store the W-foil without contamination for long time.     

Determination of iron and lead by flame atomic absorption spectrometry after preconcentration with sepiolite

By using a new adsorbent (sepiolite) an adsorption-elution and atomic absorption spectrometric method has been developed for the preconcentration and determination of Fe and Pb. Recoveries of the analytes were 82 ± 3% for Fe and 91 ± 2% for Pb at 95% confidence level. For Cu it was only 5 ± 1%. The recovery of iron could be increased to about 97 ± 1% by complexing with EDTA, the recovery of copper only to 57 ± 2%. The optimised method was applied to the determination of lead in metal materials (e.g. brass). Received: 20 February 1996 / Revised: 7 May 1996 / Accepted: 11 May 1996     

Determination of silver in environmental samples by tungsten wire preconcentration method-electrothermal atomic absorption spectrometry

A preconcentration method for silver in environmental waters involving adsorption on a tungsten wire, followed by electrothermal atomic absorption spectrometry with a tungsten tube atomizer is described. The optimal immersing time was 90 s. The best pH for the adsorption of silver was 3. Under the optimal conditions, the detection limit for silver by the tungsten wire preconcentration method was 5.0 ng l⁻¹ (3S/N) and the relative standard deviation was 8.2%. The effects of large amounts of concomitants on the preconcentration of silver were evaluated. Even though 10³- to 10⁴-fold excess of matrix elements existed in water, the silver response was not significantly affected by the matrix elements. The method with preconcentration on a tungsten wire was applied to the determination of silver in waters and proved to be sensitive, simple, and convenient. This adsorption method can be utilized in in situ sampling of ultra-trace silver in environmental samples (waters). Furthermore, after sampling it is easy to carry and store the tungsten wire without contamination for a long time.     

Determination of mercury by atomic absorption spectrometry using a platinum-lined graphite furnace for in situ preconcentration

Mercury in water samples was reduced by tin(II) chloride and the generated vapour swept in a flow of argon through a platinum-lined graphite tube to permit in situ preconcentration. Subsequent atomization of the mercury was then carried out under essentially gas-stop conditions to maximize sensitivy. The system was optimized with respect to argon gas flow and time of mercury generation/deposition using response surface methodology. Synthetic sea-water samples were analysed to test the applicability of the method. For 50-ml sample volumes, detection limits below 2 ng 1^?1 mercury could be obtained, based on twice the standard deviation of the blank. The most favourable aspect of the procedure is its simplicity, since the mercury generator can be easily constructed and connected to commonly available graphite furnace atomic absorption spectrometers.     

Determination of copper and cadmium by atomic absorption spectrometry with electrochemical and sorption preconcentration

A method is proposed for the determination of copper and cadmium by atomic absorption spectrometry in a propane-butane-air flame with electrochemical and sorption preconcentration. Electrochemical preconcentration was performed on metal (tantalum, titanium, molybdenum, and platinum), glassy-carbon, and spectrographic graphite electrodes. Sorption preconcentration was performed on filter paper with immobilized dithizone, 8-hydroxyquinoline, and rubeanic acid. It is demonstrated that copper and cadmium can be determined in water within the concentration range 1–10 ώg/L.     

Determination of total chromium in fresh water by atomic absorption spectrometry following flotation preconcentration

A flotation method is proposed for the quantitative preconcentration and determination of total chromium by electrothermal atomic absorption spectrometry in fresh water samples, without previous reduction or oxidation of the chromium ion state. Hydrated iron(III) oxide and iron(III) tetramethylenedithiocarbamate were used as precipitating collectors. The detection limit of the method is 0.01 g/L.     

浊点萃取-火焰原子吸收光谱法测定催化剂中痕量钯的研究

研究了以1-（2-吡啶偶氮）-2-萘酚（PAN）为络合剂,以非离子型表面活性刺Triton X-100为萃取剂的浊点萃取分离富集-火焰原子吸收光谱法测定痕量钯的新方法。详细考察了溶液的pH、络合剂和表面活性剂浓度、平衡温度和时间等条件对浊点萃取效果的影响。该方法对钯的检出限为30．8ng／mL,相对标准偏差（RSD）为2．1％（n=10）,回收率在97．8％-106．6％之间。可用于催化剂中Pd（Ⅱ）的测定。     

Dispersive liquid-liquid microextraction preconcentration of palladium in water samples and determination by graphite furnace atomic absorption spectrometry

A new method for the determination of palladium was developed by dispersive liquid-liquid microextraction preconcentration and graphite furnace atomic absorption spectrometry detection. In the proposed approach, diethyldithiocarbamate (DDTC) was used as a chelating agent, and carbon tetrachloride and ethanol were selected as extraction and dispersive solvent. Some factors influencing the extraction efficiency of palladium and its subsequent determination, including extraction and dispersive solvent type and volume, pH of sample solution, concentration of the chelating agent and extraction time, were studied and optimized. Under the optimum conditions, the enrichment factor of this method for palladium reached at 156. The detection limit for palladium was 2.4 ng L⁻¹ (3σ), and the relative standard deviation (R.S.D.) was 4.3% (n = 7, c = 1.0 ng mL⁻¹). The method was successfully applied to the determination of trace amount of palladium in water samples.