IR- und Raman-Spektren einiger Kaliumpentafluorometallate-monohydrate

The IR- and Raman Spectra of several compounds of the stoichiometryM ₂ ^I M ^IIIF₅H₂O and their deuterated analogs have been interpreted on the basis of their crystal structures. The compounds studied were divided into two classes regarding the bonding of water molecules. The main spectroscopic difference between the two classes was found in the region of H₂O vibrations in good agreement with theoretical predictions. The metal—fluorine and metal—oxygene vibrations gave no direct information concerning the two types of water.     

Interactions of silver halide sols with hydrolyzed hafnium species

Summary Coagulation and reversal of charge effects of freshly prepared and heated solutions of hafnium tetrachloride have been studied as a function of the p_H using aged silver halide sols and solsin statu nascendi. It was shown that the critical coagulation concentration and the critical stabilization concentration (due to charge reversal) increased with increasing p_H. These observations have been related to the hydrolysis of the hafnium ion. At p_H values above 4 essentially the entire amount of hafnium is present in the form of the neutral soluble, species Hf(OH)₄. This accounts for the inability of the hafnium solutions to reverse the charge of the sols at higher p_H values. The adsorption measurements carried out with the aid of the radioactive isotope¹⁸¹Hf showed that the neutral hydrolyzed species are strongly adsorbed on negatively charged silver iodide particles. The adsorbed amounts of hafnium on a AgI sol are considerably larger than in the case of charged hydrolyzed ions (such as hydrolyzed thorium ions) on a similar sol. This is explained by the ability of the neutral hafnium species, Hf(OH)₄. to form a close-packed adsorbed layer. The results confirm previous findings that the enhanced adsorption of hydrolyzed ions is caused by the presence of the hydroxyl group, whereas the ionic charge plays a negligible role in this case.

---

Zusammenfassung Die Koagulations- und Umladungserscheinungen von frisch dargestellten und durch Erwärmung gealterten Lösungen von Hafniumchlorid wurden an Silberhalogenid-Solen in der Abhängigkeit vom p_H untersucht. Es wurde festgestellt, daß die kritische Koagulationskonzentration und die kritische Stabilisationskonzentration (die Umladungsgrenze) mit steigendem p_H höher werden. Diese Beobachtungen wurden durch die Hydrolyse des Hafnium-Ions erklärt. Wenn p_H>4 ist, bestcht nahezu die ganze Menge von Hafnium als neutrale, gelöste Hf(OH)₄ Moleküle. Damit wird es erklärt, daß die Silberhalogenid-Teilchen bei höheren p_H-Werten durch Hafniumsalze nicht umgeladen werden können. Die mittels des radioaktiven Isotopen¹⁸¹Hf durchgeführten Messungen zeigten, daß die neutralen Hf(OH)₄ — Moleküle stark an den negativ geladenen Silberjodid-Teilchen adsorbiert sind. Die adsorbierte Menge per Mol von AgI ist beträchtlich größer als die Menge der geladenen, hydrolysierten Ionen (wie z. B. ThOH³⁺), die an dem gleichen Sol bestimmt wurde. Dieser Effekt ist leicht erklärt, da man mit den neutralen adsorbierten Molekülen eine fest gepackte Adsorptionsschicht bilden kann. Diese Resultate bestätigen die früheren Befindungen, daß die höhere Adsorptionsfähigkeit der hydrolysierten Ionen durch die Hydroxylgruppe verursacht wird, während die Ionenladung eine zu vernachlässigende Rolle spielt.

---

---

Supported by the U.S. Army Research Office (Durham), Grant No. DA-ARO (D)-31-124-G 656.

---

Part of a PhD Thesis byL. J. Stryker, supported by a NASA Traineeship.     

Mercury(II) complex with terpyridine: structure of the 2∶1 solvate of [Hg(terpy)2](CF3SO3)2 with acetone

[Hg(terpy)₂](CF₃SO₃)₂·0.5(CH₃)₂CO crystallizes in the triclinic space group witha=14.631(6),b=15.258(4),c=18.785(7) Å, =69.66(2), =70.72(1), =88.55(1)°. The crystal structure consists of two independent [Hg(terpy)₂]²⁺ cations, four trifluoromethanesulfonate anions and an acetone molecule in the asymmetric unit. Each mercury atom is coordinated by two tridentate terpyridine ligands forming an irregular six-coordination polyhedron. The Hg–N bond lengths range from 2.27(2) to 2.53(2) Å.     

Radon and gamma-radiation measurements in schools on the territory of the abandoned uranium mine “Žirovski vrhl”

On the territory of the abandoned uranium mine irovski vrh, Slovenia, indoor radon and gamma dose rate measurements were carried out in nineteen schools from February 10 to May 10, 1995, using scintillation cells and etched track detectors for radon and thermoluminescence dosimeters for gamma-ray detection. In five schools indoor radon levels exceeded 400 Bq·m^-3, which is the proposed Slovene action level. The maximum average radon value of 1600 Bq·m^-3 and the maximum gamma-dose rate of 172 Sv·month^-1 were found in the same school. According to the ICRP 65 methodology, annual effective doses from radon decay products ranged from 0.05 to 6.10 mSv for pupils and from 0.04 to 4.90 mSv for teachers. Gamma dose rates ranged from 0.05 to 0.19 mSv·y^-1 for pupils and from 0.07 to 0.27 mSv·y^-1 for teachers.     

Analytische Aspekte der Oxydation organischer Stickstoffverbindungen mit Chromsäure. XXVIII

Zusammenfassung Die schon früher beschriebene gasvolumetrische Methode zur N-N-Gruppenbestimmung durch Oxydationsaufschluß mit Chromsäure wurde zur Bestimmung des heterocyklischen Stickstoffes in Indazolinonderivaten mit Erfolg benützt und dadurch weiter die allgemeine Anwendbarkeit der Methode bestätigt. Enthält die Substanz gleichzeitig Amino- oder Nitrogruppen, können diese aus derselben Einwaage als Ammoniak bzw. Salpetersäure bestimmt werden.

---

Analytical aspects of the oxidation of organic nitrogen compounds with chromic acid

Summary The gas volumetric method for determining N-N groups by oxidative fusion with chromic acid (which has already been described previously) was successfully employed to determine the heterocyclic nitrogen in indazolinone derivatives. The general applicability of the method was thereby confirmed. If the substance contains amino or nitro groups at the same time, these can be determined in the same sample as ammonia or nitric acid.

---

---

XXVII. Mitteilung, siehe¹.     

Argentometric determination of iodide and cyanide using a depolarisation end-point

It has been shown that the depotarisation end-point technique, based on the phenomenon of a sudden out-of-balance current, produced by the establishment of a new redox potential at the indicator electrode in a pre-balanced circuit, can also be applied to precipitation titrations. The use of a platinum indicator electrode instead of one made of silver, and determination in very dilute solution, yield better results than those obtained using the classical potentiometric method.     

High-performance liquid radiochromatography: Its application for stability study of [3H] stobadin

An HPLC method was developed for studying the stability of [³H] stobadin stored in physiological saline or buffers at various pH. Optimum conditions for the separation of degradation products were elaborated. A high-performance liquid chromatograph equipped with a radioactivity detector was used.     

Recovery and recrystallization in AISI 321 steel under static conditions

Static softening of AISI 321 steel after cold and hot deformation characterizing the industrial thermomechanical treatment was studied by means of tensile tests and TEM. The deformation temperature, the strain and the grain size were the main parameters determining the final softening. The results can be applied for optimization of the solution annealing.     

Spektroskopische Untersuchungen der Metallkomplexe des 2,5-Dibenzoyl-3,4-dihydroxyselenophens

Zusammenfassung Eine Reihe von Metallkomplexen des 2,5-Dibenzoyl-3,4-dihydroxy-selenophens wurden spektroskopisch untersucht. Das Verhalten des Wismutkomplexes und die Möglichkeiten einer spektrophotometrischen Wismutbestimmung auf diesem Wege wurden eingehend studiert.

---

Summary A spectroscopic examination was made of a series of metal complexes of 2,5-dibenzoyl-3,4-dihydroxyselenophen. The behavior of the bismuth complex and the possibilities of a spectrophotometric method of determining bismuth in this manner were studied thoroughly.

---

---

Herrn Univ.-Prof. Dr.Hans Lieb zum 80. Geburtstag gewidmet.