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.     

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.     

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.     

Atomic Absorption Spectrophotometric Investigation and Determination of Palladium

This work aims to achieve a determinate characterization of compound formation and to find out the resolution to overcome chemical interferences in atomic absorption spectrophotometric (AAS) determination of palladium. The effect of flame composition in producing a neutral palladium atoms was investigated. A new analytical procedure has been elaborated for the determination of palladium.     

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。     

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.     

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.     

钯、铑和铂的同时分光光度测定

贵金属混合物光度分析常需分离,同时测定的报导亦少见。本文提出了一种不用分离,不用萃取,不用解联立方程,灵敏、简便同时分光光度测定三种贵金属的方法。     

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.     

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.     

Spectrophotometric determination of palladium with 5,6-dimethyl-1,3-indanedione-2-oxime

A rapid, sensitive and selective method has been developed for the determination of palladium with 5,6-dimethyl-1,3-indanedione-2-oxime in acetate buffer (pH 5.5). Beer's law is obeyed over the range 0.15-4.17 mug/ml palladium(II). The molar absorptivity at 370 nm is 2.98 x 10(4) 1.mole(-1).cm(-1). The method has been applied for the determination of palladium in synthetic mixtures corresponding to PtIr and Oakay alloys. An interesting feature of the system is the abnormal shape of the Job and molar-ratio plots obtained.     

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.     

氢氧化钠沉淀分离铜、钯的动力学研究及分析应用

进行了氢氧化钠沉淀分离铜钯的动力学研究,计算了用该法分离铜钯对测定引起的误差,将该法用于测定乙醛催化剂中的钯含量,获得满意结果。     

Substoichiometric determination of traces of palladium by neutron-activation analysis

A highly selective, rapid one-step radiochemical separation procedure for palladium has been developed. It is based on the solvent extraction of palladium diethyldithiocarbamate from a 5M hydrochloric acid solution with a substoichiometric amount of copper diethyldithiocarbamate in chloroform. The separation has been applied to the determination of traces of palladium by neutron-activation analysis, in platinum, the rocks W-1 and PCC-1 and a biological material (kale). Amounts of palladium down to 10(-8) g have been determined.     

Determination of Palladium Using Hydroxylamine Hydrochloride as Metal Precipitant

An analytical investigation on the quantitative reduction of palladium (II) to the metal with hydroxylamine hydrochloride in alkaline medium has been carried out. Accurate and reproducible results for the gravimetric determination of 3 to 30 mg of palladium have been recorded. Effects of various foreign metal ions on the determination have been studied.     

Extractive separation and spectrophotometric determination of palladium and platinum with dithizone in the presence of stannous chloride

The conditions [acid used, presence of chloride and tin(II)] for the extractive separation and spectrophotometric determination of palladium and platinum as the dithizonates Pd(HDz)(2) and Pt(HDz)(2) have been examined. In the absence of stannous chloride platinum does not undergo extraction. Conditions for the separation and determination of these metals in the presence of mercury, gold and copper, which are also extracted with dithizone into carbon tetrachloride or chloroform under the conditions suitable for palladium (1M sulphuric acid/0.1M hydrochloric acid), have been defined. The mercury and gold dithizonates are formed quickly and can be removed before the palladium and platinum compounds have had time to form. They can be decomposed with iodide. Copper dithizonate is decomposed by reduction with tin(II). The proposed procedure has been applied to the determination of palladium in technical platinum metal.     

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．     

Synthesis of N-o-methylphenyl-N'-(sodium p-aminobenzene-sulfonate) thiourea and its chromogenic reaction with palladium(II).

A new chromogenic reagent, N-o-methylphenyl-N'-(sodium p-aminobenzenesulfonate)thiourea (MSAT), has been synthesized and characterized by elemental analysis, (1)H-NMR, FT-IR and UV-Vis spectra. Based on the absorption spectrum of the colored complex of MSAT with palladium(II), a novel spectrophotometric method for the determination of palladium has been developed. In a pH 4.0 - 5.5 HAc-NaAc buffer solution, palladium(II) reacted with MSAT to form a stable yellow water-soluble complex with an apparent molar absorptivity of epsilon = 2.04 x 10(5) L mol(-1) cm(-1) at the maximum absorption of 318.0 nm. Beer's law was obeyed in the concentration range of 1.2 - 11.8 microg per 25 mL for palladium(II) with a correlation coefficient of 0.9997. The probable interfering ions and their tolerable limits have also been investigated in detail. The proposed method is simple, rapid, and sensitive, and has been applied to the determination of palladium in anode mud and ore samples with satisfactory results.     

Spectrophotometric determination of palladium using 4-methyl-l ,2-cyclohexanedionedioxime

A procedure for the determination of palladium with 4-methyl-1,2-cyclohexanedionedioxime by an extraction -spectrophotometric method has been developed. Interference by coppcr(II), cobalt(Il), iron(II), or iron(III) can be eliminated by suitable masking agents. Ruthenium(III) must be absent or separated prior to the determination of palladium. The molar absorptivity of the bis(4-methyl-1,2-cyclohexanedionedioximato-N,N') palladium(II) complex has been calculated and found to be 1.51?10⁴ 1/moles-cm in chloroform at 280 mμ.     

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%.