New calibrations and time stability of the response of the INTERCAST CR-39

We present new calibrations of different production batches (from 1989 to 1999) of the INTERCAST CR-39, using the BNL-AGS 1 A GeV iron beam. The comparison with previous results, obtained with the 158 A GeV lead beam from the CERN-SPS shows that, while each production batch has a different calibration curve (mainly due to minor differences in the production conditions), the aging effect is negligible. We also tested the dependence of the CR-39 response from the time elapsed between exposure and analysis (fading effect). The fading effect, if present, is less then 10%. It may be compatible with the experimental uncertainties on the bulk etching rate v_B.     

Reduction of interferences in graphite furnace atomic absorption spectrometry by multiple linear regression modelling

The multivariate effects of Na, K, Mg and Ca as nitrates on the electrothermal atomisation of manganese, cadmium and iron were studied by multiple linear regression modelling. Since the models proved to efficiently predict the effects of the considered matrix elements in a wide range of concentrations, they were applied to correct the interferences occurring in the determination of trace elements in seawater after pre-concentration of the analytes. In order to obtain a statistically significant number of samples, a large volume of the certified seawater reference materials CASS-3 and NASS-3 was treated with Chelex-100 resin; then, the chelating resin was separated from the solution, divided into several sub-samples, each of them was eluted with nitric acid and analysed by electrothermal atomic absorption spectrometry (for trace element determinations) and inductively coupled plasma optical emission spectrometry (for matrix element determinations). To minimise any other systematic error besides that due to matrix effects, accuracy of the pre-concentration step and contamination levels of the procedure were checked by inductively coupled plasma mass spectrometric measurements. Analytical results obtained by applying the multiple linear regression models were compared with those obtained with other calibration methods, such as external calibration using acid-based standards, external calibration using matrix-matched standards and the analyte addition technique. Empirical models proved to efficiently reduce interferences occurring in the analysis of real samples, allowing an improvement of accuracy better than for other calibration methods.     

Uncertainties of mercury determinations in biological materials using an atomic absorption spectrometer – AMA 254

 The method is based on catalysed ignition of a sample portion in a flow of oxygen, capture of mercury by an amalgamator and measurement of the mercury vapour's absorbance after thermic release from the amalgamator. Three powdered food samples, a certified reference material (CRM) human hair and a reference material (RM) urine (liquid) were measured in the first range of the instrument (the possible contents determined according to our measurement procedure were 0.0003–0.5 ppm). The calibration function used was a line passing through the origin. The combined standard uncertainties of the mercury determinations were computed from uncertainty components of five quantities: absorbance of the sample, absorbance of the sample blank, slope of the calibration line, correction factor of the abscissa axis, and mass or volume of the sample. The most important uncertainty component is the uncertainty of the sample absorbance measurement which amounts to 52% of the determination uncertainty at the minimum (RM urine) and about 90% at the maximum (in our laboratory homogenized powdered food samples; analysis of variance showed their homogeneity to be insufficient). The results of the CRM and RM analyses do not indicate a significant systematic error for this determination. The relative expanded uncertainty (coefficient was 2) of the determination increases from 9 to 13% for the insufficiently homogenized samples with decreasing mercury content (range of 0.004–0.03 ppm); higher homogeneity of samples results in a decrease of the expanded uncertainty, e.g. 4.6% for the liquid sample (RM urine). Received: 26 April 1999 / Accepted: 30 August 1999     

Optical 3-D dynamic measurement system and its application to polymer membrane inflation tests

An optical surface measurement system, which is capable of measuring transient surface shape, has been developed by using a high-speed digital camera. The system is based on the grating projection and Fourier transform technique. A calibration procedure is developed to allow the system to generate Cartesian coordinates directly, which are with respect to a fixed coordinate system in 3-D space. The measurement accuracy (±50 μm) is defined and verified as the maximum error between measured values and the known values of standard objects both flat and curved. The camera and a grating projector are mounted into a portable sensor head to allow in situ measurements. In addition, external force or pressure signals can be correlated with each measurement through a device called the multi-channel data link. The system is capable of digitizing a 3-D curved surface into an array of points with known xyz coordinates at a sampling rate from 30 to 1000 Hz. As an application, the system is used to measure the transient surface shape during a polymer membrane inflation test. The measurement results along with the pressure information provide an approach to determine the material parameters used in different material models.     

Modelling tire-moist terrain interaction using advanced computational techniques

This paper focuses on predicting and analyzing the tire-moist terrain interaction. The moist terrain (sand) is modelled using Smoothed-Particle Hydrodynamics (SPH) technique. The SPH basic interpolation technique is described, and the necessary interpolation equations are implemented. The soil is modelled using the hydrodynamic elastic-plastic material, while the water is modelled using Murnaghan equation of state. The numerical interaction between both materials is defined using Darcy’s law. The soil moisturizing technique consists of layering water particles on top of sand particles and pressurizing the water into the sand. The moisturizing technique is examined using the direct shear-strength test, and validated against physical measurement carried out in a laboratory under similar soil conditions and bulk density. Finally, the results and the effect of moisture content on tire-moist terrain interaction are discussed and investigated using a previously modelled and validated off-road truck tire size 315/80R22.5.     

The construction of simultaneous optimal experimental designs for several polynomials in the calibration of analytical methods

In this paper a criterion is described for the construction of experimental designs for the evaluation of calibration models in analytical chemistry. The proposed criterion seeks a compromise between the D-optimal designs for estimating the parameters of different polynomial models. A computer algorithm is presented for a sequential construction of experimental designs using the optimality criterion. The performance of the optimality criterion and the computer algorithm is elaborated for the problem of discrimination between a first- to a third-degree polynomial for the calibration of analytical methods. An experimental design consisting of replicate measurements at five distinct levels equally spaced over the calibration range proved a good solution.