Extractive Spectrophotometric Determination Of Palladium Research Articles

Extractive spectrophotometric determination of palladium with N, N, N′, N′-tetra(2-ethylhexyl)- thiodiglycolamide T(2EH)TDGA

A precise, sensitive and selective method for the spectrophotometric determination of palladium (II) using N, N, N′, N′-tetra(2-ethylhexyl) thiodiglycolamide T(2EH)TDGA as an extractant is described. Palladium (II) forms yellow colored complex with T(2EH)TDGA which exhibits an absorption maximum at ∼300 nm. The colored complex obeys Beer's law in the concentration range 1.0–15.0 μg ml −1 of palladium with a molar absorptivity of 1.29 × 10 5 M −1 cm −1. The effects of various experimental parameters have been studied to establish the optimum conditions for the extraction and determination of palladium. The precision of the method has been evaluated and the relative standard deviation has been found to be less than 0.5%. The method has been successfully applied to the determination of palladium in simulated high level liquid waste (SHLW) solution.

Synthesis of New Reagent Benzyloxybenzaldehydethiosemicarbazone (BBTSC): Selective, Sensitive and Extractive Spectrophotometric Determination of Pd(II) in Water Samples and Synthetic Mixtures

AbstractA new reagent, benzyloxybenzaldehydethiosemicarbazone (BBTSC) was synthesized and a new method was developed for the simple, highly selective and extractive spectrophotometric determination of palladium(II) with BBTSC at wave length 365 nm. The metal ion formed a yellow colored complex with BBTSC in acetate buffer of pH 5.0, which was easily extractable into cyclohexanol with 1:1 (Metal: Ligand) composition. The method obeys Beer's law in the range of 5–60 ppm. The molar absorptivity and Sandell's sensitivity were found to be 0.4 × 104 Lt. mol−1 cm−1 and 0.02661 μg cm−2, respectively. The correlation co‐efficient of the Pd(II)‐BBTSC complex was 0.9657, which indicated an excellent linearity between the two variables. The repeatability of the method was checked by finding the relative standard deviation (RSD) (n = 10), which was 0.321% and its detection limit 0.016875 μg.mL−1. The instability constant of the method was calculated by Asmus' method as 3.5714 × 10−4. The interfering effect of various cations and anions were also studied. The proposed method was successfully applied for the determination of palladium(II) in synthetic and water samples. The results were compared with those obtained using an atomic absorption spectrophotometer, testing the validity of the method.

Selective and sensitive extractive spectrophotometric determination of micro amounts of palladium(II) in spiked samples: using a new reagent N-ethyl-3-carbazolecarbaxaledehydethiosemicarbazone

N-Ethyl-3-cabazolecarboxaldehydethiosemicarbazone (ECCT) is proposed as a new, sensitive and selective complexing reagent for the separation and extractive spectrophotometric determination of palladium(II) at pH: 4.0 to form a yellowish orange colored 1:1 chelate complex, which is very well extracted in to n-butanol. The absorbance was measured at a maximum wavelength, 410 nm. This method obeys Beer's law in the concentration range 0.0-6.6 microg mL(-1) and the correlation coefficient of Pd(II)-ECCT complex is 0.998, which indicates an excellent linearity between the two variables with good molar absorptivity and Sandell's sensitivity, 1.647 x 10(4) l mol(-1)cm(-1), 6.49 x 10(-3) microg cm(-2), respectively. The instability constant of complex calculated from Edmond's method, 2.724 x 10(-5) was in good agreement with the value calculated from Asmus' method 2.624 x 10(-5), at room temperature. The precision and accuracy of the method is checked with calculation of relative standard deviation (n = 5), 0.839. Edmond's method was observed to be a more selective method in the presence of EDTA, oxalate and phosphate ions. The method was successfully applied for the determination of Pd(II) in water samples, synthetic mixtures and hydrogenation catalysts, employing an atomic absorption spectrometer for comparing these results.

Highly sensitive extractive spectrophotometric determination of palladium(II) in synthetic mixtures and hydrogenation catalysts using benzildithiosemicarbazone.

A simple and highly sensitive method was developed for the extractive-spectrophotometric determination of palladium with benzilidithiosemicarbazone. The metal ion formed a reddish brown complex with benzildithiosemicarbazone in a potassium chloride-hydrochloric acid buffer of pH 2.5, which was easily extractable into methyl isobutyl ketone. The 1:1 complex showed the maximum absorbance at 395 nm with a Beer's law range of 0.25-3.5 ppm. The molar absorptivity and Sandell's sensitivity were found to be 3.018 x 10(4) dm3 mol(-1) cm(-1) and 0.0035 microg cm(-2), respectively. The correlation coefficient of the Pd(II)-BDTSC complex was 0.998, which indicated an excellent linearity between the two variables. The repeatability of the method was checked by finding the relative standard deviation (RSD) (n = 10), which was 0.46%. The instability constant of the complex calculated from Edmond and Birnbaum's method was 2.41 x 10(-5), that of Asmus' method is 2.53 x 10(-5) at room temperature. The interfering effects of various cations and anions were studied. The proposed method was successfully applied to the determination of palladium(II) in synthetic mixtures and hydrogenation catalysts. The validity of the method was tested by comparing the results with those obtained using an atomic absorption spectrophotometer.

A rapid and sensitive extractive spectrophotometric determination of palladium(II) in synthetic mixtures and hydrogenation catalysts using pyridoxal-4-phenyl-3-thiosemicarbazone.

A rapid and sensitive extractive spectrophotometric method has been developed for the determination of palladium(II) in synthetic mixtures and hydrogenation catalysts using pyridoxal-4-phenyl-3-thiosemicarbazone (PPT) as an analytical reagent. The reagent forms a red-color complex with the metal at pH 3.0, which is extracted into benzene. The absorbance is measured at 460 nm. The method adheres to Beer's law up to a concentration range of 0.4-6.4 microg cm(-3). The molar absorptivity and Sandell's sensitivity are 2.20 x 10(4) dm3 mol(-1) cm(-1) and 4.85 x 10(-3) microg cm(-2), respectively. The correlation coefficient of the Pd(II)-PPT complex is 0.99, which indicates an excellent linearity between two variables. The detection limit of this method is 0.05 microg cm(-3). The instability constant of the Pd(II)-PPT complex calculated from Edmond and Birnbaum's method is 2.90 x 10(-5) and that of Asmus' method is 2.80 x 10(-5) at room temperature. The concurrent repetition of the method is checked and the relative standard deviation (RSD) (n = 5) was derived as 1.84 percent. The present method was applied to the determination of palladium(II) in synthetic mixtures and hydrogenation catalysts. The results were compared by employing an atomic-absorption spectrometer.

Stopped-flow injection liquid–liquid extraction spectrophotometric determination of palladium in airborne particulate matter and automobile catalysts

A stopped-flow injection liquid–liquid extraction (SF-EX-FIA) spectrophotometric method is reported for the determination of palladium(II), using the 2,2′-dipyridyl-2-pyridylhydrazone (DPPH) as a color forming reagent. The colored complex Pd(II)–DPPH was extracted in CHCl 3 and the absorbance was monitored at 560 nm. An injection valve was used as a commutator in order to combine the stopped-flow technique with liquid–liquid extraction FI system. The calibration graph was linear up to 12 mg l −1 ( s r=0.27%; r=0.9999) with a detection limit of c L=0.007 mg l −1. The sampling rate was 20 injections per hour. The proposed method has been successfully applied to the determination of palladium in airborne particulate matter (APM) and in automobile exhaust gas converter catalysts.

Extraction-Spectrophotometric Determination of Palladium with 3-Thiophenaldehyde-4-phenyl-3-thiosemicarbazone

A highly selective spectrophotometric method is described for the determination of palladium, using 3-thiophenaldehyde-4-phenyl-3-thiosemicarbazone (TAPS). The method is based on the formation of an insoluble palladium(II)-TAPS complex, which is extractable into chloroform from 1 M sulfuric acid medium after shaking for 10 min. The complex system conforms to Beer′s law over the concentration range 0.4-6 μg ml −1 of palladium. The proposed method has been satisfactorily applied to the determination of palladium in brazing filler metals.

Extractive spectrophotometric determination of palladium from acidic high activity nuclear waste

A simple and rapid method for spectrophotometric determination of palladium from highly acidic and highly radioactive nuclear waste using α-benzoin oxime (ABO) as extractant and isobutyl methyl ketone (hexone) as diluent has been developed. The method can be employed over a wide range of nitric acid concentrations and for palladium concentrations in the range of 1·10−5M to 4·10−4M in the organic phase. The molar absorptivity was found to be 4·103l·mol−1·cm−1. Influence of various heavy metal ions, fission products and corrosion products was studied. The method was found to give a precision and accuracy better than 4% at 100 μg of palladium.

Extractive spectrophotometric determination of palladium using 2-(2-hydroxyimino-1-oxoethyl)furan

A rapid, simple, selective and sensitive method for the determination of palladium in trace amounts has been developed, based on the reaction of 2-(2-hydroxyimino-1-oxoethyl)furan [α-isonitroso-2-acetyl-furan] with the metal ion in acetic acid. The intense yellow complex is quantitatively extractable into chloroform, whose absorbance is measured at 425 nm. The method is free from the interference of a large number of other metal ions. It obeys Beer's law in the range 0.0–3.8 μg Pd mL−1 with Sandell's sensitivity of 0.003 μg Pd cm−2. The ratios of metal to ligand in the extracted complex are 1:1 and 1:2. The analysis of various samples has been carried out with satisfactory and reproducible results.

Diphenylthiovioluric Acid as a Sensitive and Selective Reagent for Extractive Spectrophotometric Determination of Palladium (II)

Diphenylthiovioluric Acid as a Sensitive and Selective Reagent for Extractive Spectrophotometric Determination of Palladium (II)

Selective Extractive Spectrophotometric Determination of Palladium (II) with Di-2-Pyridyl Ketone 2-Pyridyl-Hydrazone (DPPH)

Abstract Palladium (II) reacts with DPPH in slightly acid medium to form a red colored complex stable in presence of EDTA and extractable into chloroform. These properties of the Pd(II)-DPPH complex were used for the selective extractive spectrophotometric determination of palladium(II) in presence of several tested cations.

Extractive Spectrophotometric Determination of Palladium with Di-2-pyridylmethanone 2-(5-Nitro)pyridylhydrazone

The spectrophotometric characteristics of the complexes formed with di-2-pyridylmethanone 2-(5-nitro)pyridylhy-drazone (DPNPH) and eight metal ions are reported. The reagent appears to be promising especially for palladium(ll) and cobalt(ll) in selectivity and for copper(ll), nickel(ll), zinc(ll) and cadmium(ll) in sensitivity. A detailed study has been made for the extractive spectrophotometric determination of up to 2.8 ppm of palladium(ll) in the presence of chloride ions. The molar absorptivity of the complex extracted into 1,2-dichloroethane is 3.78x104 I mol-1 cm-1 at 560 nm. The method is satisfactorily applied to the determination of palladium in some palladium catalysts.

Simultaneous extractive spectrophotometric determination of palladium(II)-platinum(II) or palladium(II)-gold(III) with benzyltriethylammonium ion and iodide in the presence of EDTA

Palladium(II), platinum(II), and gold(III) react with benzyltriethylammonium ion and iodide in slightly acid medium to form water-insoluble colored ternary complexes stable in the presence of EDTA and extractable into MIBK. Palladium(II)-platinum(II) and palladium(II)-gold(III) can be determined simultaneously in the presence of several cations by the proposed method.

Extractive spectrophotometric determination of palladium(II) in dental alloys with 3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine and tetrabromophenolphthalein ethylester.

A sensitive spectrophotometric method for the determination of Pd(II) in dental alloys is proposed. It is based on the reaction of 3-(2-pyridyl)-5, 6-diphenyl-1, 2, 4-triazine (PDT) and Pd(II) and on the formation of a 1:1 ion associate with tetrabromophenolphthalein ethylester (TBPE) which is extractable into 1, 2-dichloroethane at pH 56. A required amount of the dental alloy sample (0.10.5 g) was dissolved in 5 ml of concentrated nitric acid by heating and the resulting solution was evaporated to dryness. The residue was dissolved again in 5 ml of 1 M hydrochloric acid by heating. The solution was filtered, and the filtrate was diluted to 100 ml with 1 M hydrochloric acid. A sample solution containing up to 10 μg of Pd was transferred into a 50 ml-volumetric flask. To it, 1 ml of 5 × 10-3 M PDT solution, 2 ml of 3 × 10-3 M TBPE solution and 15 ml of buffer solution (pH 5.5) were added and the mixture was diluted to 50 ml with distilled water. After standing for 10 min, the solution was transferred into separatory funnel. It was shaken with 10 ml of 1, 2-dichloroethane for 10 min. After the organic phase was centrifuged to remove droplets of water, absorbance of the organic phase was measured at 610 nm against the reagent blank. The calibration curve was linear over the range 20200 ppb of Pd(II) and the apparent molar absorptivity was 10.8 × 104 1 mol-1 cm-1; Sandell sensitivity, 0.00098 μg cm-2; and the standard deviation, 1.5%. Although Co(II), Fe(II), Cu(II), Rh(III) and Ru(II) interfered with the determination of Pd(II) in the general procedure, these interferences could be reduced by adding appropriate masking agents.

Extractive spectrophotometric determination of palladium(II) and platinum(II) with 2-allylthiourea and thiocyanate in the presence of EDTA

Palladium(II) and platinum(II) react with 2-allylthiourea and thiocyanate to form colored complexes stable in the presence of EDTA and extractable into isoamyl alcohol. Based on these properties a method was worked out for the extractive spectrophotometric determination of palladium(II) and platinum(II) in the presence of several cations.

An extraction-spectrophotometric determination of palladium with 4-(2-pyridylazo)resorcinol in the presence of diphenylguanidine

A new, sensitive spectrophotometric determination of palladium has been developed, based on the extraction of the red Pd(II) chelate with 4-(2-pyridylazo)resorcinol in the presence of N,N′-diphenylguanidine into n-butanol; the sensitivity of the method according to Sandell is S = 1.12 μg cm −2, ϵ 530 = 9.4 × 10 4 liters mol −1 cm −1, and palladium can be determined at concentrations from 0.21 to 1.91 μg ml −1.

Extraction-Spectrophotometric Determination of Palladium(H) with Di-2-pyridyl Ketone Benzoylhydrazone

A method for the extractive spectrophotometric determination of palladium(II) with di-2-pyridyl ketone benzoylhydrazone (DPKBH) has been studied. The method is based on the formation of the palladium(II)-DPKBH complex which is extracted into benzene from sulfuric acid solution in the presence of chloride ions. The extracted species has absorption maxima at 455 and 481nm with the molar absorptivity of 9.38×103 Lmol-1 cm-1 at the former wavelength. Beer′s law is obeyed over the range 0-10μg ml-1 of palladium at 455nm. The proposed method is selective in the presence of tartaric or citric acid and has been satisfactorily applied to the determination of palladium in a dental alloy and in palladium-catalyst samples.

Separation and extractive spectrophotometric determination of palladium and platinum with 6-aminoquinoxaline-2,3-dithiol

Separation and extractive spectrophotometric determination of palladium and platinum with 6-aminoquinoxaline-2,3-dithiol

Liquid-liquid extraction and spectrophotometric determination of palladium(II) and ruthenium (III) with isonitrosoethylbenzoylacetate

A method is described for the extractive spectrophotometric determination of palladium or ruthenium (III) using isonitrosoethylbenzoylacetate as the reagent. The yellow Pd-INEBA complex extracted into chloroform absorbs at 410 nm and conforms to Beer's law in the range of 10–110μg of Pd per 10 ml of organic phase. The purple Ru-INEBA complex extracted into MIBK absorbs at 500 nm and conforms to Beer's law in the range of 25–125μg of Ru per 10 ml of organic phase. The method affords the determination of both Pd and Ru in the presence of large number of cations and anions.

2,2'-Dipyridyl-2-quinolylhydrazone as a reagent for the spectrophotometric determination of metals: The extractive spectrophotometric determination of palladium(II)

2,2'-Dipyridyl-2-quinolylhydrazone, DPQH, is proposed as a Spectrophotometric reagent for certain metal ions. The composition, extractability and Spectrophotometric characteristics of the complexes formed with 7 metal ions are reported. DPQH appears to be promising especially for palladium(II) and cobalt(II) in selectivity and for zinc(II) and cadmium(II) in sensitivity. A detailed study has been made for the extractive spectrophotometric determination of palladium(II) in the presence of chloride ions.