Standardization of Methods for Characterizing the Surface Geometry of Solids

Since a comprehensive survey published in 1999 [1] much work was done in standardizing measuring methods to characterize the surface geometry of dispersed and/or porous solids and to certify reference materials. The present paper is an extension of a short communication [2]. It gives a survey on existing standards and reports on new drafts and proposals.     

Extension of the measuring range of balances

The basic principle of comparing the sample mass with the mass of a reference body in equilibrium gives the equal-armed beam balance a unique accuracy. Main parameters characterising the suitability of the instrument are measuring range, resolution and relative sensitivity (resolution/maximum load). The historical development of the values of these parameters achieved depended strongly on the practical need in those times. Technically unfavourable scales of the oldest Egyptian dynasties (~3000 BC) could resolve mass differences of 1 g and had a relative sensitivity of at least 10^–3. More sophisticated instruments from the 18^th Dynasty (~1567–1320 BC) achieved a relative sensitivity of 10^–4 independent of the size of the instrument. In 350 BC Aristotle clarified the theory of the lever and at about 250 BC Archimedes used the balance for density determinations of solids. The masterpiece of a hydrological balance was Al Chazini’s 'Balance of Wisdom’ built about 1120. Its relative sensitivity was 2⋅10^–5. Real progress took place when scientists like Lavoisier (1743–1794) founded modern chemistry. At the end of the 19^th century metrological balances reached a relative sensitivity of 10^–9 with a maximum load of several kilogrammes. That seems to be the high end of sensitivity of the classical mechanical beam balance with knife edges. Improvements took place by electrodynamic compensation (Emich, Gast). In 1909 Ehrenhaft and Millikan could weigh particles of 10^–15 g by means of electrostatic suspension. In 1957 Sauerbrey invented the oscillating quartz crystal balance. By observing the frequency shift of oscillating carbon nanotubes or of silica nanorods, masses or mass changes in the attogram or zeptogram have been observed recently.     

General application of jäntti's method for the fast calculation of sorption equilibrium

On the basis of a molecular model for adsorption kinetics Jäntti introduced a method to calculate equilibriums shortly after a change of the pressure of the sorptive gas. In the present paper we show that this method is useful in many more situations than those intended originally.     

Comments on surface structure analysis by water and nitrogen adsorption

Specific surface area and pore size distribution are determined usually from adsorption isotherms at low temperatures using nitrogen or noble gases. These are not absolute parameters and the measuring methods are fraught with serious difficulties. General problems of sorption measurements and recent developments are discussed. To obtain information for practical purposes these measurements need to be supplemented by investigations of the sorbate/sorbent system used in practice. Results of the measurement of nitrogen and water vapour adsorption on different materials are compared. This revised version was published online in July 2006 with corrections to the Cover Date.     

The characterization of the capability of a balance

A survey is given on important standardized definitions by which the capability of balances may be characterized. Some modifications are proposed with regard to the use of mass sensors for the continuous determination of mass variations. An important supplement is the relative resolution introduced by Jenemann. Optimum values are presented.I am indepted to H. R. Jenemann for his critical remarks.     

Application of jäntti's method to volumetric adsorption measurements

Jäntti introduced a method to calculate the adsorption equilibrium by measuring the actual adsorbed amount three times after a change to the gas pressure. By this method the experimental time for adsorption measurement can be considerably shortened. The procedure was developed for use in adsorption measurements where the adsorbed masses are directly measured with a balance. In the present paper we will demonstrate that the method is particularly useful in volumetric (manometric) measurements.     

Estimation of the dimensions of nano-capillaries from gas adsorption data

A new approach is presented to determine the dimensions of cylindrical nanopores from adsorption measurements.     

Considerations on the planned use of a scientific balance on Mars

The balance is the most widely used complex measuring instrument in science and techniques. To install a balance on Mars is a challenge for numerous aspects of in situ measurements in the next decade. By means of a balance useful parameters could be determined and a variety of investigations could be carried out there. Possible applications of a balance on Mars are reviewed. Choice of type and demands on the balance with regard to the conditions on Mars are discussed. The first step is to test a load cell with strain gauge deflection sensor.     

Calorimetric investigation of the vulcanization of factice

Sulphur factice is produced from a mixture of a vegetable oil and sulphur at temperatures between 130 and 160C. The slow exothermal vulcanization results in rubber-like elastomers. We have developed an isothermal calorimeter for measurements both in the liquid and the solid state and simulated the production process at the laboratory scale. The compensating calorimeter consists of a hot plate equipped with thin aluminium rods descending into a Dewar vessel. Besides optimization of the temperature control, remarkable savings of time were achieved by previous elaidinization of the oil using hydrosulphide.

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Zusammenfassung Schwefeffaktis wird aus einer Mischung von pflanzlichem öl und Schwefel bei Temperaturen zwischen 130 und 160C hergestellt. Ein langsamer, exothermer Vulkanisierungsprozess führt zu gummiÄhnlichen Elastomeren. Es wurde ein isothermes Kalorimeter entwickelt für Messungen sowohl im flüssigen als auch festen Zustand und damit der Herstellungsprozess im Laboratoriumsma\stab simuliert. Das Kompensations-Kalorimeter besteht aus einer heizbaren Platte, die mit dünnen, sich in ein DewargefÄ\ erstreckenden AluminiumstÄben versehen ist. Neben einer Optimierung der Temperaturkontrolle lie\en sich betrÄchtliche Zeiteinsparungen erzielen, indem das öl zuvor durch Behandlung mit Schwefelwasserstoff bei Temperaturen zwischen 120 und 300C elaidiniert wurde.

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The investigation was performed at Battelle-Institute e.V. Frankfurt am Main. The authors highly appreciated the valuable discussions with Dr. Lohmann (D. O. G.) and Dipl.- Ing. R. Nowack (Battelle). We are indebted to the D. O. G. Deutsche ölfabrik Ges. f. Chem. Erz. mbH & Co., Hamburg, for financial support.     

Studies of heterogeneity properties of selected high-temperature superconductor surfaces

Nitrogen adsorption measured at 77 K was used to characterize the surface heterogeneity of high-temperature superconductor surfaces. Properties relating to adsorption and porosity of the solids (adsorption capacity, specific surface area, radii and volume of the pores, pore-size distribution function) were determined from nitrogen adsorption–desorption isotherms and atomic force microscopy (AFM) for a series of oxide superconductors. It is shown that the adsorption isotherms of all samples are S-shaped and belong to type II according to the IUPAC classification. On the basis of the nitrogen adsorption isotherms and AFM data, fractal dimensions were determined and correlations found with adsorption and porosity parameters.