• Journal of the Korean Chemical Society
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• v.15 no.4
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• pp.191-197
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• 1971

Ruthenium content in highly purified palladium metal (99.9%) was determined by counting $^{105}Rh$ nuclide which was produced by $^{104}Ru(n,{\gamma};{\beta}^-)^{105}Rh$ nuclear reaction. Palladium sample and ruthenium standard were irradiated by neutron with the Pneumatic Transfer System of TRIGA MARK II reactor. Palladium and ruthenium were dissolved by treating with aqua-regia and by fusing with sodium peroxide flux respectively. $^{105}Rh$ was separated through anion and cation exchange resin columns. The ruthenium content was determined by comparing the $^{105}Rh$ activities, obtained from the palladium sample, with that from pure ruthenium standard. The detection limit of ruthenium by the present method is about 1 ppm of ruthenium in 10 mg of palladium, which is approximately 40 times more sensitive than that of the conventional radioactivation method which employs $^{102}Ru(n,{\gamma})^{103}Ru$ nuclear reaction.

• Bulletin of the Korean Chemical Society
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• v.21 no.1
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• pp.56-60
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• 2000

The mechanism of a matrix modification for the trace determination of volatile lead and bismuth by an electro-thermal atomic absorption spectrophotometry was studied by a X-ray diffractometry (XRD). For the investigation of structures, the ash products of the elements were produced by using a palladium as a matrix modifier with or without aluminum or nickel as an auxiliary modifier. The same charring conditions as in the analysis of samples were applied together with much concentrated solution of analytical elements and modifiers in a graphite furnace to get a large amount of the product for XRD. The XRD patterns showed PbPd3 for lead and BiPd3 for bismuth. These mean that the reaction procedures through the charring and atomization were changed from $Pb^{2+}$ ${\rightarrow}$ PbO ${\rightarrow}$$Pb^0$ to $Pb^{2+}$ ${\rightarrow}$ PbO ${\rightarrow}PbPd_3$ ${\rightarrow}$ Pb o for lead and from $Bi^{3+}$ ${\rightarrow}$ BiO ${\rightarrow}$ Bi o to $Bi^{3+}$ ${\rightarrow}$ BiO ${\rightarrow}$ $BiPd_3$ ${\rightarrow}$ $Bi^0$ for bismuth by the addition of modifiers. The volatile elements were stabilized by the formation of palladium alloys through a charring process. Charring temperatures were raised about 500 $^{\circ}C$ by the alloying and the atomization was also stabilized for the enhancement of sensitivities.

• Journal of the Korean Chemical Society
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• v.36 no.2
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• pp.243-247
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• 1992

Inductively coupled plasma-atomic emission spectrometry was applied to determine the palladium in $SnO_2$ employed for a gas sensor. Since $SnO_2$ is hardly decomposed into the solution, extensive studies were devoted to the development of decomposition methods which minimize the interference effect. The matrix effects on the background level and emission intensity of the element were studied and they were compensated by using matrix matched solution.

• Journal of the Korean Chemical Society
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• v.40 no.2
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• pp.109-116
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• 1996

A matrix modification was studied for the determination of trace germanium in mineral waters by electrothermal atomic absorption spectrophotometry (ET-AAS). For this, the type and quantity of modifier as well as the use of auxiliary modifier were investigated to realize the efficient modification. Germanium suffers from low sensitivity and poor reproducibility in ET-AAS determination because of the premature loss of germanium via volatile germanium monoxide formation when heated in the presence of carbon. Therefore, the addition of a matrix modifier is necessary to stablize the germanium, thermally and chemically. By the addition of palladium (10 ${\mu}g/mL)$ as a single modifier to the sample containing 500 ng/mL germanium, the charring temperature could be raised from 800 to $1000^{\circ}C$, and its absorbance was also increased, but the atomization temperature was not raised. In this case, the absorbance of germanium was not changed in the range of 10∼70 ${\mu}g/mL$ of palladium added. On the other hand, it was considered that the use of a mixed modifier could modifiy the matrix more effectively than with a single modifier. The best results were obtained by using 1% ammonium hydroxide as an auxiliary modifier together with 10 ${\mu}g/mL$ palladium. The charring temperature could be raised from 800 to $1100^{\circ}C$, without any change of the atomization temperature. With above optimum conditions, the trace amount of germanium in several mineral waters were determined by a calibration curve method, and good recoveries of more than 95% were also obtained in the samples in which a given amount of germanium was spiked. The detection limit of this method was about 6.9 ng/mL.

• Journal of the Korean Chemical Society
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• v.39 no.3
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• pp.204-212
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• 1995

The graphite furnace atomic absorption spectrophotometric determination of trace lead in water samples was studied using matrix modifiers. In order to modify the sample matrix, the type and optimum amount of the modifier were investigated with a given concentration of Pb solution. In fact, if the matrix is not modified, lead has low ashing and atomization temperatures as to give a low absorbance with bad reproducibility because of its volatility. Therefore, optimum modifiers should be used to stabilize the atomization. In this work, the ashing and atomization temperatures were raised from 400 and $1800^{\circ}C$, to 1,000 and $2000^{\circ}C$, by the addition of palladium to 50 ng/mL lead solution as a modifier. The concentration of palladium was 5.0 ${\mu}g/mL$ in the modified solution. Furthermore, if 1.5 ${\mu}g/mL$ of aluminum was mixed with the palladium modifier as an auxiliary modifier, the ashing temperature could be increased $150^{\circ}C$ additionally. With such a treatment, the sensitivity was improved more than 5 times of the solution unmodified and the reproducible results of less than 5% RSD were obtained in the samples of university's waste water and pipe-washing tap water. It could be concluded that this procedure was quantitative in the determination of trace lead from the recoveries of more than 88% obtained in the samples in which a given amount of lead was spiked.

• Analytical Science and Technology
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• v.8 no.4
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• pp.691-698
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• 1995

The complexation of platinum and palladium with synthetic polyelectrolytes was studied. The successive and overall stability constants of Pd(II) with PEI and 2PVP were obtained by potentiometric titration. Because of the slow equilibrium time, the potentiometric titrations were performed using the home-made automatic titrator in order to analyze the complexations according to the modified Bjerrum method. The complex formation constant of Pt(IV) with 2PVP, measured by differential pulse polarography, was calculated from the peak currents that were obtained in non-complexing media and in solution containing 2PVP.

• Polymer(Korea)
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• v.39 no.3
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• pp.487-492
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• 2015

The effects of chemical structure of alkyl groups of norbornene carboxylic alkyl esters(methyl, octyl, 4-chlorobenzyl) and endo/exo ratios of norbornene monomers on activity of palladium catalyst and polymerization behavior were investigated. Norbornene ester monomers were synthesized from the reaction of 5-norborene-2-carboxylic acid and various alcohols. Polymerization catalyst, di-${\mu}$-chloro-bis(-methoxybicyclo[2,2,1]-hept-2-ene)palladium(II) (DCBMP), was synthesized according to the literature procedure and silver hexafluoroantimonate ($AgSbF_6$) was used as a conjugate anion source. Gel permeation chromatography (GPC), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) were the principal techniques for polymer characterization and $^1H$ NMR spectroscopy was used for chemical structures determination of monomers and polymers. For all of the norbonene alkyl esters GPC data showed that when the amounts of endo isomers exceeded those of exo isomers decreased molecular weight polymers were obtained probably due to the decreased catalyst activity. Polymerizations were conducted by varying the monomer/catalyst mole ratios (100:1, 200:1, 300:1). When 300:1 monomer/catalyst ratio was employed it was possible to synthesize high molecular weight ($M_n=27500g/mol$), film forming polymer from exo-norbornene carboxylic acid octyl ester.

• Transactions of the Korean hydrogen and new energy society
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• v.7 no.1
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• pp.111-115
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• 1996

Metal atom rearrangement has been shown to take place under the influence of hydrogen-induced atomic diffusion (HIAD) in initially homogeneous fee palladiumalloys by electron microprobe analysis, optical microscopy, mechanical property tests and hydrogen isotherms. HIAD takes place in palladium alloys at moderate to elevated temperatures leading to phase segregation under conditions where segregation does not normally occur, i.e., in the absence of H over the time scale of the experiments. From these results, it is confirmed that dissolved hydrogen plays a dual role in some of these alloys, i.e. it catalyzes metal atom diffusion. This research demonstrates the potential utility of employing H-induced changes for phase diagram determination of Pd alloys and possibly for other alloy system.

• Analytical Science and Technology
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• v.12 no.2
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• pp.130-135
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• 1999

A graphite furnace atomic absorption spectrometry (GFAAS) with matrix modification has been used to determine trace amounts of arsenic, lead and selenium in rice flour samples. A mixed solution of palladium and magnesium nitrate was used as a matrix modifier to convert the analyte elements into a phase of higher thermostability and to increase the volatility of concomitants in graphite furnace. Matrix modification effects by the mixed solution were investigated for several elements (As, Cd, Cu, Pb, Se, Zn). It has been found that the matrix modifier substantially increase the pyrolysis and atomization temperature, and absorbance for As, Pb and Se. The concentration of As, Pb and Se in rice flour samples were determined by standard addition method with Zeeman background correction after microwave acid digestion. In this method the characteristic concentrations of As, Pb and Se are 26 ng/g, 18 ng/g, 24 ng/g on the basis of dry sample respectively.

• Analytical Science and Technology
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• v.13 no.5
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• pp.608-615
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• 2000

A determination method of trace nickel and cobalt in water samples was studied and developed by adsorbing their complexes on ion exchange resin suspension. The analytical ions were formed as complexes with a ligand of APDC (ammonium pyrrolidinedithiocarbamate) and adsorbed on anion exchange resin of Dowex 2-X8. After the suspension was filtered out with membrane filter, the complexes were dissolved in HCl solution by an ultrasonic vibrator for ET-AAS determination. Several conditions were optimized as followings. pH of sample solution: 5.0, amount of ligand APDC: more than 430 times in mole ratio, the type and concentration of acid: 0.1 M HCl, and vibration time: 7 minutes. The addition of palladium in the HCl solution could improve the reproducibility and sensitivity by a matrix modification in the absorbance measurement. This procedure was applied for the analysis of three kinds of real water samples. The detection limits equivalent to 3 times standard deviation of blank were Co 0.36 ng/mL and Ni 0.27 ng/mL and recoveries in spiked samples were 99-102% for cobalt and 100-105% for nickel.