The use of ethylenediaminetetraacetic acid or nitrilo-triacetic acid as masking agents in the determination of palladium with dimethylglyoxime or quinaldic acid

The use of complexing agents to mask interference in the gravimetric determination of palladium has been studied. Ethylenediaminetetraacctic acid was used to complex interfering ions in the determination of palladium with dimethylglyoxime, and nitrilotriacetic acid has been employed as a masking agent in the determination of palladium with quinaldic acid. From 15 to 150 mg of palladium were determined. All the metals tested do not interfere with the exception of gold which s reduced by the complexing agents and has to be removed prior to the determination. The procedures are rapid, simple and accurate.     

催化动力学光度法测定痕量钯

在磷酸－磷酸二氢钾缓冲溶液中，以钯（Ⅱ）催化次磷酸钠还原罗丹明Ｂ褪色为指示反应，建立了痕量钯的动力学光度分析新方法。在金（Ⅱ）的存在下，检测下限达５×１０＾－１１ｇ／ｍＬ钯（Ⅲ），方法应用于模拟合金样和含钯分子筛中钯的测定。结果满意。     

Zero-crossing second derivative spectrophotometry for simultaneous determination of palladium and nickel using 1-(2-pyridylazo)-2-naphthol in mixed micellar solutions

1-(2-Pyridylazo)-2-naphthol (PAN) has been used for the simultaneous determination of nickel and palladium at trace levels. PAN complexes of nickel and palladium in the pH 1.98 form red and green colored complexes, respectively, which are soluble in aqueous 4:1 Triton X-100 to sodium dodecylsulfate (SDS) micellar media with total detergent concentration of 3.2%. Under optimum conditions, calibration graphs for the simultaneous determination by second derivative spectrophotometry were obtained. Zero crossing second derivative spectrophotometry at 668 and 572 nm, respectively for palladium and nickel was used for the simultaneous determination. The method is able to determine palladium to nickel ratio 70:1 to 1:6 (Wt/Wt), accurately. Accuracy and reproducibility of the determination method on the known various amounts of palladium and nickel in their binary mixtures were tested. Effects of diverse ions on the determination of palladium and nickel to investigate selectivity of the method also were studied.     

Simultaneous spectrophotometric determination of mercury and palladium with Thio-Michler's Ketone using partial least squares regression and orthogonal signal correction

A simple, novel and sensitive spectrophotometric method was described for simultaneous determination of mercury and palladium. The method is based on the complex formation of mercury and palladium with Thio-Michler's Ketone (TMK) at pH 3.5. All factors affecting on the sensitivity were optimized and the linear dynamic range for determination of mercury and palladium found. The simultaneous determination of mercury and palladium mixtures by using spectrophotometric method is a difficult problem, due to spectral interferences. By multivariate calibration methods such as partial least squares (PLS), it is possible to obtain a model adjusted to the concentration values of the mixtures used in the calibration range. Orthogonal signal correction (OSC) is a preprocessing technique used for removing the information unrelated to the target variables based on constrained principal component analysis. OSC is a suitable preprocessing method for PLS calibration of mixtures without loss of prediction capacity using spectrophotometric method. In this study, the calibration model is based on absorption spectra in the 360-660 nm range for 25 different mixtures of mercury and palladium. Calibration matrices were containing 0.025-1.60 and 0.05-0.50 microg mL(-1) of mercury and palladium, respectively. The RMSEP for mercury and palladium with OSC and without OSC were 0.013, 0.006 and 0.048, 0.030, respectively. This procedure allows the simultaneous determination of mercury and palladium in synthetic and real matrix samples good reliability of the determination.     

Substoichiometric determination of traces of palladium by radioactive isotope-dilution analysis

A radioactive isotope-dilution method for the determination of traces of palladium has been developed. It is based on the solvent extraction of palladium dithizonate from acid solution by means of a substoichiometric amount of dithizone in carbon tetrachloride. The separation has been applied to the determination of traces of palladium in platinum, the rocks W-1 and PCC-1 and a biological material (kale). Amounts of palladium down to 3 ng have been determined.     

H-point standard addition method--first derivative spectrophotometry for simultaneous determination of palladium and cobalt

H-point standard addition method (HPSAM) has been applied for simultaneous determination of palladium and cobalt in trace levels, using disodium 1-nitroso-2-naphthol-3, 6-disulphonate (nitroso-R salt) as a selective chromogenic reagent. Palladium and cobalt in the neutral pHs form red color complexes with nitroso-R in aqueous solutions and making spectrophotometric monitoring possible. Simultaneous determination of palladium and cobalt were performed by HPSAM--first derivative spectrophotometry. First derivative signals at the two pairs of wavelengths, 523 and 589 nm or 513 and 554 nm were monitored with the addition of standard solutions of palladium or cobalt, respectively. The method is able to accurately determine palladium/cobalt ratio 1:10 to 15:1 (wt/wt). Accuracy and reproducibility of the determination method on the various amounts of palladium and cobalt known were evaluated in their binary mixtures. To investigate selectivity of the method and to ensure that no serious interferences were observed the effects of diverse ions on the determination of palladium and cobalt were also studied. The recommended procedure was successfully applied to real and synthetic cobalt or palladium alloys, B-complex ampoules, a palladium-charcoal mixture and real water matrices.     

Simultaneous Laser Thermal Lens Spectrometric Determination of Trace Platinum and Palladium in an Aquesous Solution

A selective and sensitive method for determination of platinum and palladium(Ⅱ）in an aqueous solution simultaneously by laser thermal lens spectrometry,based on the complex reaction of 2-(3,5-dichloropyridylazo)-5-dimethylaminoamiline(3,5-diCl-PADMA) with platinum and palladium,has been developed.It is shown that the palladium complex can be fromed at room temperature, while the platinum complex can be only formed after being heated in a boiling water bath.By using this difference of reaction temperature and the characteristic of the complexes mentioned above,the method for simultaneous determination of platinum and palladium was established in an aqueous solution without a pre-separation.The results show that the dynamic linear ranges of determination for platinum and palladium are 0.005-0.04μg/mL and 0.005-0.25μg/mL respectively,and that the detection limits are both 0.002/μg/mL.The method has been applied to the determination of platinum and palladium simultaneously in alloy and catalyst samples with satisfactory results.     

Amperometric determination of palladium with 2-(o-Hydroxyphenyl) Benzoxazole

Summary A method for the amperometric determination of palladium is presented, which involves the formation of a palladium-2-(o-hydroxyphenyl) benzoxazole inter complex salt. The method is primarily recommended for the accurate determination of palladium in solutions containing only traces of other platinum elements. Of the several diverse ions studied, only iridium interfered seriously with the determination of palladium; however, this element is easily removed from palladium according to the standard procedure². The data obtained in the amperometric investigation of the palladium-2-(o-hydroxyphenyl) benzoxazole interaction were in agreement with the results obtained in the gravimetric study of the same reaction⁷.     

H-Point Standard Addition Method for Simultaneous Determination of Palladium and Cobalt

The H-point standard addition method (HPSAM) has been applied to simultaneous determination of palladium and cobalt at trace levels, using 1-(2-pyridylazo)-2-naphthol (PAN) as a chromogenic reagent. Palladium and cobalt at neutral pH levels form green colored neutral complexes with PAN which are soluble in aqueous sodium dodecylsulfate (SDS) micellar media and can be monitored spectrophotometrically. Simultaneous determination of cobalt and palladium by HPSAM were performed spectrophotometrically and under optimum conditions. Absorbances at the two pairs of wavelengths, 597 and 650 nm or 566 and 612nm, were monitored while adding standard solutions of cobalt or palladium, respectively. The method is able to accurately determine a cobalt/palladium ratio of between 5:1 and 1:30 (wt/wt). The accuracy and reproducibility of the determination method for various known amounts of cobalt and palladium in their binary mixtures were evaluated. The effects of diverse ions on the determination of cobalt and palladium to investigate the selectivity of the method were also studied. The recommended procedure was applied to real water samples and synthetic sample solutions.     

Optimization of a chemical modifier in the determination of selenium by graphite furnace atomic absorption spectrometry and its application to wheat and wheat flour analysis.

A method for the determination of total selenium in wheat and wheat flour using graphite furnace atomic absorption spectrometry (GFAAS) with palladium/ascorbic acid as a chemical modifier was studied. The effects of nickel nitrate, palladium/ascorbic acid, and palladium/magnesium nitrate as chemical modifiers on the sensitivity in the determination of selenite, selenate and selenomethionine by GFAAS were compared. The palladium/ascorbic acid modifier was used for the determination of total selenium in wheat and wheat flour, because the oxidation states of the selenium ion are not important in the determination. The detection limit was estimated to be 1 microg L(-1) (calculated as 3sigma of the blank); the calibration curve was linear for the concentration range 5 - 50 microg L(-1) and the recovery range was 96.66 - 101.80%. The optimal ashing and atomizing temperatures were 1300 degrees C and 2250 degrees C, respectively. The proposed method was successfully applied to the determination of total selenium in wheat and wheat flour.     

Second and first-derivative spectrophotometry for efficient simultaneous and individual determination of palladium and cobalt using 1-(2-pyridylazo)-2-naphthol in sodium dodecylsulfate micellar media.

1-(2-Pyridylazo)-2-naphthol (PAN) has been used for the simultaneous and individual determination of palladium and cobalt at trace levels. PAN complexes of palladium and cobalt at neutral pH form green-color neutral complexes, which are soluble in aqueous SDS micellar media. Under optimum conditions, calibration graphs for individual determinations by zero and first-derivative spectrophotometry, and also for simultaneous determinations by second-derivative spectrophotometry were obtained. A zero-crossing method using second-derivative spectrophotometry at 628 or 578 and 614 nm, respectively, for cobalt and palladium was used for simultaneous determinations. The method is able to determine the cobalt-to-palladium ratio, 5:1 to 1:10 (Wt/Wt), accurately. The accuracy and reproducibility of the determination method for various known amounts of cobalt and palladium in their binary mixtures were tested. The effects of diverse ions on the determination of cobalt and palladium to investigate the selectivity of the method were also studied. The recommended procedures were applied to a synthetic binary alloy, cobalt in vitamin B12 and B-complex ampoules, a Co2O3-Co3O4 laboratorial chemical mixture, some synthetic cobalt-alloy samples, a Pd-charcoal catalyst, and some synthetic palladium alloys.     

Sorption–Spectrometric Determination of Palladium in Chloride Solutions

A sorption–spectrometric method was developed for the determination of palladium in solutions of complex composition using cellulose filters impregnated with trioctylamine with the subsequent formation of the colored compound of palladium with 4-(2-pyridylazo)resorcinol on the filter. It was demonstrated that conditions for the preconcentration of palladium coincide with conditions for the formation of colored compounds (green and red forms of palladium complexes) in the sorbent phase. The highest selectivity is observed for the formation of the green form; in this case, the determination of palladium is not affected by the interference from large amounts of concomitant elements (macrocomponents of ores). Palladium was determined on filters by diffuse reflectance spectrometry with the calculation of chromaticity characteristics and by a test scale. The detection limits were 0.5 (green form) and 0.3 (red form) g of palladium on the filter. High precision of results of the determination of palladium (RSD < 5%) is attained in a wide range of its concentrations.     

Amperometric titration of palladium, silver and copper with benzimidazol-2-ylmethanethiol, and its application to non-ferrous materials

A method is described for the determination of mg amounts of palladium, silver and copper by amperometric titration with benzimidazol-2-ylmethanethiol in acetate buifer medium (pH 4-5) at an applied potential of -0.2 V vs. the saturated calomel electrode. Direct titrations are possible in the presence of a number of foreign ions. Copper and palladium interfere mutually and in the determination of silver. Mercury(I), mercury(II) and platinum(IV) also interfere. Silver does not interfere in the determination of copper and palladium if it is first precipitated as chloride. The method has been successfully applied to the analysis of non-ferrous materials.     

Gravimetric and spectrophotometric determination of palladium with 2,3,4-pentanetrione trioxime

A study of the use of 2,3,4-pentanetrione trioxime (PTT) in the gravimetric and spectrotrophotometric determination of palladium is reported. PTT has been applied to the determination of palladium in various synthetic and standard samples. The reagent has some advantages over dimethylglyoxime.     

Determination of Palladium by Graphite Furnace Atomic Absorption Spectrometry After Preconcentration with MCI GEL CHP 20P Resin as Sorbent

A solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of palladium with MCI GEL CHP 20P resin as sorbent was studied. Trace amounts of palladium was reacted with 2-ethylhexyl octyl sulfide followed by adsorption onto MCI GEL CHP 20P solid phase extraction column, and ethanol was used as eluent. The enrichment factor of this method for palladium was reached at 250. The detection limit in the original sample for palladium was found to be 0.0048 ng mL^?1. The proposed method has been successfully applied to the determination of trace amounts of palladium in different samples.     

Kinetic spectrophotometric determination of trace amounts of palladium by whole kinetic curve and a fixed time method using resazurine sulfide reaction

The univariate and multivariate calibration methods were applied for the determination of trace amounts of palladium based on the catalytic effect on the reaction between resazurine and sulfide. The decrease in absorbance of resazurine at 602 nm over a fixed time is proportional to the concentration of palladium over the range of 10.0-160.0 ng mL(-1). The calibration matrix for partial least squares (PLS) regression was designed with 14 samples. Orthogonal signal correction (OSC) is a preprocessing technique used for removing the information unrelated to the target variables based on constrained principal component analysis. OSC is a suitable preprocessing method for PLS calibration without loss of prediction ability using spectrophotometric method. The root mean square error of prediction (RMSEP) for palladium determination with fixed-time, PLS and OSC-PLS were 3.71, 2.84 and 0.68, respectively. This procedure allows the determination of palladium in synthetic and real samples with good reliability of the determination.     

5-（5-溴-2-吡啶偶氮）-2，4-二氨基甲苯催化光度法测定钯

在H2SO4介质和室温条件下,微量钯（Ⅱ）对KBrO3氧化5-（5-溴-2-吡啶偶氮）-2,4-二氨基甲苯（5-Br-PA—DAT）褪色反应具有显著的催化作用,据此建立了测定微量钯的催化光度法．方法的检测限为0．034mg／L,线性范围0．2～0．75mg／L．已用于钯碳催化剂及水样中钯含量的测定,标准加入回收率为97．2％～99．0％,结果满意．     

新试剂5-(5-碘-2-吡啶偶氮)-2,4-二氨基甲苯高选择性分光光度法测定微量Pd(Ⅱ)

研究了新试剂5-(5-碘-2-吡啶偶氮)-2,4-二氨基甲苯(5-I-PADAT)与Pd(Ⅱ)的显色反应。实验结果表明,在0.6～1.8mol/L高氯酸介质中,于室温下放置10min,Pd(Ⅱ)与5-I-PADAT可形成1∶1蓝紫色络合物,其最大吸收波长位于583nm,表观摩尔吸光系数ε为7.2×104L·mol-1·cm-1,Pd(Ⅱ)的浓度在0～1.0μg·mL-1符合比耳定律。由于反应直接在强酸性介质中进行,而在此酸度下,其它金属离子几乎不能反应,因此具有极高的选择性。所拟方法操作简单、快速,可应用于合金、矿样和分子筛中微量钯的测定。     

Gravimetric determination of palladium with 2-(o-Hydroxyphenyl) benzoxazole

Summary A method has been developed for the direct gravimetric determination of palladium. The method saves time and is reproducible and accurate. Of the several cations and anions studied, only a few of the cations interfered seriously with the determination of palladium.     

The application of deuterium-palladium electrodes in the coulometric-potentiometric determination of bases in ketone media

The application of deuterium-palladium electrodes as generator, indicator and reference electrodes for the determination of organic bases in acetone and methyl ethyl ketone has been investigated. Deuterium dissolved in palladium is oxidized at a potential that is close to the oxidation potential of hydrogen in palladium and more negative than the oxidation potentials of the bases titrated, indicator, and the solvents used. The anodic oxidation of deuterium dissolved in palladium proceeds with 100% current efficiency in the solvents investigated. The relative errors for the determination of 5 x 10(-4)M solutions of bases are less than 1%.