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  • Articles  (45)
  • Spektralphotometrie  (24)
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  • Articles  (45)
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  • Springer  (45)
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  • 1
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    Journal of nondestructive evaluation 2 (1981), S. 57-63 
    ISSN: 1573-4862
    Keywords: ultrasonics ; correlation ; pseudorandom codes ; random signals ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract A new portable digital random signal flaw detection system is described which uses a digital delay line to replace the acoustic delay line of the original random signal system. Using this new system, a comparison was made between the two types of transmit signals which have been used in previous systems—m-sequences and random signals. This comparison has not been possible with these previous correlation flaw detection systems. Results indicated that for high-speed short code operation, the m-sequences produced slightly lower range sidelobes than typical samples of a clipped random signal. For normal long code operation, results indicated that system performance is essentially equivalent in resolution and signal-to-noise ratio using either m-sequences or clipped and sampled random signals. Further results also showed that for normal long code operation, the system produces outputs equivalent in resolution to pulse-echo systems, but with the added benefit of signal-to-noise ratio enhancement.
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  • 2
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    Journal of nondestructive evaluation 2 (1981), S. 85-111 
    ISSN: 1573-4862
    Keywords: Holographic reconstruction ; ultrasound ; NDE ; Rayleigh-Sommerfeld formula
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract For the purpose of ultrasonic nondestructive testing of materials, holography in connection with digital reconstruction algorithms has been proposed as a modern tool to extract crack sizes from ultrasonic scattering data. Defining the typical holographic reconstruction algorithm as the application of the scalar Kirchhoff diffraction theory to backward wave propagation, we demonstrate its general incapability of reconstructing equivalent sources, and hence, geometries of scattering bodies. Only the special case of a planar measurement recording surface, that is to say, a hologram plane, and a planar crack with perfectly rigid boundary conditions parallel to the hologram plane and perpendicular to the incident field yields a nearly perfect correlation between crack size and reconstructed image; the reconstruction algorithm is then referred to as the Rayleigh-Sommerfeld formula; it therefore represents the optimal case matched to that special geometrical situation and, hence, may be interpreted as a quasi-matched spatial filter. Using integral equation theory and physical optics, we compute synthetic holographic data for a linear cracklike scatterer for both plane and spherical wave incidence, the latter case simulating a synthetic aperture impulse echo situation, thus illustrating how the Rayleigh-Sommerfeld algorithm or its Fresnel approximation increasingly fail for cracks inclined to the hologram plane and excited nonperpendicularly. Furthermore, we point out how the physical data recording process may additionally influence the reconstruction accuracy, and, finally, guidelines for a careful and serious application of these holographic reconstruction algorithms are given. The theoretical results are supported by measurements.
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  • 3
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    Journal of nondestructive evaluation 2 (1981), S. 203-207 
    ISSN: 1573-4862
    Keywords: ultrasonics ; synthetic aperture ; spatial frequency ; interior imaging ; acoustic microscopy ; defect detection ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract A new acoustic synthetic aperture geometry is demonstrated in which the image field is sampled in the spatial frequency domain. This means the sampled field is recorded in a particularly convenient form for presentation to the back propagation algorithms used to reconstruct the field at the object plane. The method has applications in interior visualization. It is difficult to image the interior of solid objects using lens based imaging systems because a different lens geometry must be used for each distinct object material. The system presented here overcomes such problems since both the angular variation of the transmission coefficient at the object-water interface and the aberrations introduced by the velocity mismatch at the object surface may be readily compensated for in the back propagation routine. Experimental results are presented illustrating the detection of four half wavelength diameter defects, spaced by three wavelengths, at a depth of eight wavelengths below the surface of an aluminum block.
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  • 4
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    Journal of nondestructive evaluation 2 (1981), S. 241-247 
    ISSN: 1573-4862
    Keywords: ultrasonic field ; numerical methods ; transducer design ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract A simple, flexible, accurate, and comprehensive numerical method is presented for theoretically analyzing the diffraction field of a continuous wave transducer of arbitrary size, shape, and frequency. Using the extensively studied circular transducer for comparison, numerical results are shown for an unfocused transducer with uniform velocity excitation as well as for a focused transducer with Gaussian velocity excitation. Data concerning the execution time, program size, and convergence of the method are also presented for its implementation as a design tool on a minicomputer system.
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  • 5
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    Journal of nondestructive evaluation 2 (1981), S. 23-33 
    ISSN: 1573-4862
    Keywords: austenitic stainless steel ; austenitic stainless steel welds ; eddy current inspection ; eddy current testing ; electromagnetic testing ; ferromagnetic steel inspection ; flaw characterization ; flaw detection ; NDE ; multifrequency eddy current inspection ; weld inspection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract This paper describes the initial phase of a project to develop eddy-current methods to inspect welds joining sections of austenitic stainless steel pipe having walls up to 13 mm (0.5 in.) thick. The objective of this phase was to demonstrate the feasibility of detecting and characterizing flaws in austenitic stainless steel base metals. These materials and welds present challenging eddy-current problems because of their relatively large thickness and ferromagnetism. Multiparameter analysis shows that a reflection coil probe operated with three discrete driver frequencies and phase detection can locate and size a cracklike defect in a single conductor in the presence of variations in conductor resistivity, permeability, and thickness and in the probe-conductor spacing (liftoff). Experiments were performed with a modular three-frequency instrument. Flat-plate specimens of types 304L and 347 stainless steel machined to 12.7 to 15.9 mm thickness simulated pipe walls; saw-cut slots 10 to 30% of nominal specimen thickness simulated cracklike defects. The same slots were used in duplicate experiments as near-side (directly under the test probe) or far-side (in the face opposite the probe) defects. Flaw detection and characterization capability was demonstrated by a series of experimental measurements fitted to specimen properties by least squares techniques. The quality of the fit determined the expected accuracy of measurement. Comparison of accuracy estimates determined the best choice of operating frequencies. From the 1,2,5 sequence of frequencies between 0.5 and 20 kHz, the optimum set of operating frequencies was selected to be 0.5, 2, and 10 kHz. Estimates of measurement accuracy for combined near- and far-side defect cases were: plate thickness, 0.74 mm; probe liftoff, 0.03 mm; defect location (depth of material above defect), 3.48 mm; and defect size (vertical slot depth), 1.09 mm. A few property values were back-calculated from instrument readings; the errors in these values were somewhat larger than the measurement accuracy estimates because of instrument drift and the absence of calibration circuits.
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  • 6
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    Journal of nondestructive evaluation 2 (1981), S. 35-41 
    ISSN: 1573-4862
    Keywords: acoustic emission ; crack growth ; 7075 aluminum ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract For slow crack growth (da/dn ≈0.1 µm per load cycle) in 7075-T6 aluminum, quantitative agreement was found between the amplitude distribution of burst acoustic emissions and the area size distribution of intermetallic inclusions ≈10 (µm)2 in area as measured on thepolished fracture face. This observation permits the prediction of the amplitude distribution of acoustic emissions due to crack growth in a particular sample of 7075-T6 aluminum directly from a simple, standard metallographic observation performed on the material in question. It was also found that a reduction of the yield stress from that of 7075-T6 aluminum (503 MPa) to that of 7075-0 aluminum (103 MPa) completely eliminated burst acoustic emission activity due to crack advance in the amplitude range studied.
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  • 7
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    Journal of nondestructive evaluation 2 (1981), S. 119-124 
    ISSN: 1573-4862
    Keywords: Stress intensity factor ; annular crack ; finite element methods ; fatigue ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract Results of finite element static stress intensity factor calculations for an annular crack around a spherical inclusion (void) are presented and compared with those from approximate analytical methods.
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  • 8
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    Journal of nondestructive evaluation 2 (1981), S. 147-149 
    ISSN: 1573-4862
    Keywords: Ultrasonic tomography ; residual stress ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract Ultrasonic tomography is being explored as a potential tool to map residual stresses in solids. The angular scanning required in tomography imposed limitations on the stress configuration adaptable to such a treatment. These are discussed in the following note.
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  • 9
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    Journal of nondestructive evaluation 2 (1981), S. 161-172 
    ISSN: 1573-4862
    Keywords: elastodynamic inverse scattering ; ultrasonics ; data reduction ; ill-posed problems ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract The practical significance of ill-posedness in a data reduction problem is reviewed. Inverse elastodynamic scattering is shown to be ill-posed in general, although suitably restricted problems may be well-posed. These results underscore the need to analyze carefully the errors of data reduction problems in NDE, and to focus attention on final results of an NDE exercise, rather than on intermediate steps.
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  • 10
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    Journal of nondestructive evaluation 2 (1981), S. 153-159 
    ISSN: 1573-4862
    Keywords: ultrasonics ; scattering ; cracks ; periodic surface perturbation ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract The scattering of a plane longitudinal wave from a two-dimensional crack, with a sinusoidal surface perturbation whose amplitude and wavelength are much smaller than the length of the crack, is investigated. The amplitude of the cylindrical body waves in the far field are calculated from a Kirchhoff approximation that utilizes the solution to the reflection from the sinusoidal surface profile of a semiinfinite solid. The results are compared to those for a flat crack, and conditions for significant differences of the amplitude as a function of the angle of observation are discussed. Characteristic changes in the scattered field produced by profiles with different amplitudes and periods are explained.
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  • 11
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    Journal of nondestructive evaluation 2 (1981), S. 195-202 
    ISSN: 1573-4862
    Keywords: ac potential difference ; fatigue crack measurement ; slots ; artificial flaws ; parasitic voltages ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract The development of a successful and accurate instrument for measuring surface-breaking cracks in metals using the ac field technique has raised several interesting theoretical problems. Measurements with the instrument, known as the Crack Microgauge, do not rely on any prior calibration against an artificial flaw such as a saw-cut in a test block, but some users accustomed to such a calibration from other devices have nevertheless wished to use the instrument in that fashion and have in some instances reported erroneous results. In this paper, we develop a simple theory to explain and quantify this phenomenon. We calculate the parasitic voltages induced in the instrument probe due to the finite opening possessed by an artificial flaw, and we use these results to reinterpret the instrument readings. Controlled experimental measurements on artificial flaws of rectangular cross-section made in aluminum and in steel are found to be in good agreement with the theory. It is shown, however, that application of the theory requires additional information about the internal phase shift associated with the instrument. To enhance the accuracy of the theory, the effect of the corners of the artificial flaws was also considered, although it was not very influential in this work.
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  • 12
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    Journal of nondestructive evaluation 2 (1981), S. 43-49 
    ISSN: 1573-4862
    Keywords: Rayleigh wave dispersion ; higher mode generation ; cold-working ; rail ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract The propagation of the Rayleigh surface wave is experimentally studied along the top surface of used railroad rail under conditions where ultrasonic pulses have carrier frequencies ranging from 0.4 to 3.0 MHz and approximately 10 µs duration. The generation of the first higher (M 21 or Sezawa) mode as well as the fundamental (M 11) mode and their dispersion properties are observed. These phenomena are attributable to the presence of the cold-worked surface layer caused by the wheel passage. It is shown that a theoretical model of a single layer overlying a half space, whose elastic constants are determined by a destructive method, yields results which agree with the dispersion curves obtained experimentally. On the basis of this one-layered model, an inversion method to estimate the layer thickness and its elastic constants is discussed.
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  • 13
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    Journal of nondestructive evaluation 2 (1981), S. 65-74 
    ISSN: 1573-4862
    Keywords: NDE ; cast iron ; vibration analysis ; modulus ; strength
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract An outline is given of the existing nondestructive vibration tests for cast irons and their drawbacks in terms of the dimensional accuracy of the components. A proposal is made for a new test based on the change of resonant frequency with vibration amplitude exhibited by cast irons. This proposal is evaluated using material data obtained from dynamic tests of a wide range of cast iron specimens. A test rig is described suitable for testing cylindrical cast bars, and typical results are presented in relation to material strength. There is also a brief description of preliminary testing on cast products.
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  • 14
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    Journal of nondestructive evaluation 2 (1981), S. 113-118 
    ISSN: 1573-4862
    Keywords: Capacitance ; dielectric constant ; voids ; cellular glasses ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract Cellular (foamed) glasses are a prime candidate for certain structural applications, such as support of the silvered glass concentrator mirrors in solar thermal energy systems. An economical nondestructive measurement of strength-limiting defects in these materials would permit development of designs in which the material is subjected to a higher working stress level and maintains the same probability of failure. This would result in weight and cost savings for any application. A method of measuring the capacitance of well-defined regions of a specimen was investigated. Large voids were found to produce significant localized changes in the capacitance of the specimen. The feasibility of locating the large, strength limiting defects in this porous material has been demonstrated for one type of cellular glass. Means of producing an image from this type of data and an implementation scheme for on-line production measurements are discussed.
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  • 15
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    Journal of nondestructive evaluation 2 (1981), S. 139-146 
    ISSN: 1573-4862
    Keywords: Material defects ; 14 MeV neutrons ; pulse-shape analyzer system ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract A 14 MeV neutron generator and fast neutron spectrometer consisting of an organic scintillation detector and a pulse-shape analyzer are used for the nondestructive testing of materials. The 14.6 MeV peak (in the 12.7–15.7 MeV region) is observed to change as a function of both the kind of testing material and the defect condition inside the material. The number of neutron counts under the 14.6 MeV peak for lighter testing materials (e.g., plastic, brass, and aluminum) with a defect will increase, as compared to the number of neutron counts under the same peak region of an identical testing material but with no defect. For heavier testing materials (e.g., steel and lead), the inverse is observed. The method is feasible even with defects of size 0.25 cm3 (i.e., a cylindrical cavity 0.4 cm in diameter and 2.0 cm in length), although quantitative evaluation of the size of the defect as a function of the change of the number of neutron counts under the 14.6 MeV peak region is difficult due to instability of the 14 MeV neutron output.
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  • 16
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    Journal of nondestructive evaluation 2 (1981), S. 219-229 
    ISSN: 1573-4862
    Keywords: acoustics ; surface acoustic waves ; Rayleigh waves ; ceramics ; surface cracks ; residual stresses ; crack extension ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract An investigation of scattering from surface cracks has been conducted. In particular, the change in the reflection coefficient of a Rayleigh wave incident on a surface indentation crack has been measured as the sample is stressed to fracture. The acoustic measurements have been correlated with the stable crack extension that precedes final failure. The crack extension behavior of as-indented specimens was found to differ appreciably from that of annealed specimens. Cracks in the annealed samples exhibited partial crack tip closure, but little stable extension, whereas cracks in the as-indented samples displayed both crack closure and irreversible crack growth. This behavior has been rationalized by invoking concepts based upon the residual stresses created by indentation.
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  • 17
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    Journal of nondestructive evaluation 2 (1981), S. 51-55 
    ISSN: 1573-4862
    Keywords: Love wave dispersion ; surface layer ; work hardening ; rail ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract In this paper, experiments show Love wave generation along the top surface of used railroad rail, where the shear wave velocity has been slightly reduced by the cold-working of wheel passage for years. The rf pulses used in the experiments have about 10 µs duration and a relatively narrow frequency spectrum. The group velocity of the Love wave is found to have a strong dependence on the carrier frequency over the tested range of 0.45–3.1 MHz. Application of the seismological one-layered model to the experimental measurements yields an NDE technique for the elastic properties and the thickness of the cold-worked surface layer. The results are interpreted on the basis of a destructive observation by micro-Vickers hardness testing.
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  • 18
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    Journal of nondestructive evaluation 2 (1981), S. 75-84 
    ISSN: 1573-4862
    Keywords: digital signal processing ; microprocessor based system ; binary display ; ordered dither ; ultrasonic C-scan ; image magnification ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract The use of a digital microprocessor based system for the acquisition of ultrasonic C-scan information is investigated. The C-scan information is displayed on a binary display device using electronic ordered dither techniques to represent gray levels. The digital system with a binary display increases system flexibility and yields better reproducibility and constant image quality independent of the display medium. Images may be stored on magnetic tape or disk for later retrieval and image processing. The techniques which are described allow for image magnification and a reduction in scan time by replacing the mechanical linkage between the scanner and the display with digital signals. A detailed comparison is made between two dither signals, and the advantages of each are discussed. The combination of digital signal processing and imaging techniques produces results which utilize the capabilities of ultrasonic inspection to the point where the transducer becomes the limiting factor.
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  • 19
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    Journal of nondestructive evaluation 2 (1981), S. 133-138 
    ISSN: 1573-4862
    Keywords: X-rays ; diffraction ; grain size determination ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract It is shown that the grain size of commercial materials can be estimated by x-rays with little or no sample preparation. The method is readily automated and can be employed on-line, for example, in a rolling mill.
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  • 20
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    Journal of nondestructive evaluation 2 (1981), S. 173-188 
    ISSN: 1573-4862
    Keywords: ultrasonics ; acoustic imaging ; computer image analysis ; failure prediction ; inhomogeneous materials ; accept/reject criteria ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract A computerized technique is presented which has been developed for analyzing acoustic images of an inhomogeneous material. The acoustic imaging system is briefly described with emphasis on its adaptation to billets of graphite for atmospheric reentry body use. Ultrasonic images of such inhomogeneous material contain a nonuniform distribution of anomalies and few, if any, geometrically regular features which can be assessed to establish material integrity. Results obtained with our new algorithms show, for certain discriminants, a high degree of correlation between the numerical accept/reject values obtained from acoustic image processing and the time-to-failure of the graphitic material in simulated atmospheric reentry tests.
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  • 21
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    Journal of nondestructive evaluation 2 (1981), S. 209-217 
    ISSN: 1573-4862
    Keywords: honeycomb panels ; acoustic inspection ; leaky waves ; SH and Lamb waves ; line scan ; NDE
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Mathematics
    Notes: Abstract This paper considers the properties of elastic waves guided by an aluminum plate bonded to a honeycomb core for application to rapid inspection of honeycomb panels. Current acoustic inspection techniques involve the transmission of a signal between a pair of small transducers located on opposite sides of the panel. Scanning the transducers in raster fashion results in a high resolution inspection of the panel, but is very time consuming. An alternative technique would simultaneously inspect all points along a line between two widely spaced transducers located on the same side of the panel. Scanning the pair once over the panel permits rapid inspection, although with decreased resolution. Studies presented here indicate that such a method of inspection is feasible and that the flexural mode is probably the most useful.
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  • 22
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    Fresenius' Zeitschrift für analytische Chemie 305 (1981), S. 413-414 
    ISSN: 1618-2650
    Keywords: Best. von Nitroparaffinen, prim. ; Spektralphotometrie ; Überf. in Hydroxamsäuren, Vanadium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 306 (1981), S. 125-128 
    ISSN: 1618-2650
    Keywords: Best. von Antimon mit Triphenyltetrazoliumchlorid ; Spektralphotometrie ; Extraktion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The optimum conditions for the antimony(V) extraction in strong hydrochloride acid medium as a ternary ion-associated complex with triphenyltetrazolium chloride have been investigated. The extraction constant has been determined with dichlorethene and chloroform (1∶1) (K ex =3.06×104). A working procedure for the determination of antimony has been developed. Interferences are only caused by iron(III), gold(III), thallium(III) and gallium. The application of the method is demonstrated by the analysis of metallic lead, which has also been carried out with two other methods (AAS and spectrophotometry with crystal violet). The new method is superior in reliability and accuracy. The relative standard deviation of the mean is ± 7.4%.
    Notes: Zusammenfassung Die optimalen Bedingungen für die Extraktion von Antimon aus stark salzsaurer Lösung als Ionenanlagerungskomplex mit Triphenyltetrazoliumchlorid wurden bestimmt. Die Extraktionskonstante bei Extraktion mit einer Dichlorethan-Chloroform-Mischung (1∶1) beträgt (K ex =3,06·104). Für die Antimonbestimmung wurde eine entsprechende Methode ausgearbeitet. Nur Fe(II), Au(III), Tl(III) und Ga(III) stören. Die Anwendung der Methode wurde an Hand der Analyse von metallischem Blei demonstriert, die zusätzlich auch nach zwei anderen Methoden (AAS und Spektralphotometrie mit Kristallviolett) durchgeführt wurde. Die neue Methode ist in bezug auf Zuverlässigkeit und Genauigkeit überlegen. Die relative Standardabweichung des Mittelwertes beträgt ± 7,4%.
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    Fresenius' Zeitschrift für analytische Chemie 306 (1981), S. 129-135 
    ISSN: 1618-2650
    Keywords: Best. von Kobalt in Cyanocobalamin, Wasser ; Spektralphotometrie ; 5-Brom-PADAP
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Eine empfindliche und selektive spektralphotometrische Kobaltbestimmung (〈0,9 μg ml−1) ist mit 2-(5-Brom-2-pyridylazo)-5-diethylaminophenol (5-Brom-PADAP) auf Grund des kinetisch stabilen Co(III)L 2 − -Chelates möglich, das nach seiner Bildung bei pH 7 (Ammoniumacetat) in Gegenwart von 0,1% Triton X-100, 5,10−3 M Ammoniumperoxodisulfat und 10% (v/v) Dimethylformamid (auch nach Zugabe von 1,25 M H2SO4, 1,80 M HNO3 oder auch 0,1–0,01 M EDTA) stabil ist. Eine Reihe von 5-Brom-PADAP-Chelaten störender Ionen werden dabei zersetzt. V(V), Hg2+, Ni2+, Cu2+, Pd2+ können stören. Die Kobaltbestimmung in Cyanocobalamin und auch Trinkwasser ist auf diesem Wege möglich. Die Fehler lagen im Bereich von — 3 bis — 7 % (1,8–9 μg Co/l).
    Notes: Summary A sensitive and selective determination of cobalt (〈0.9 μg ml−1) with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Bromo-PADAP) is carried out at pH7 in the presence of ammonium acetate buffer, 5×10−3M ammonium peroxodisulphate, 0.1% Triton X-100 and 10% (v/v) dimethylformamide. The kinetically inert Co(III)L 2 − chelate, if once formed at pH 7 is stable over a broad pH interval for a certain period (in 1.25 M H2SO4, 1.80 M HNO3 or 0.1–0.01 M EDTA, where many other 5-Bromo-PADAP chelates are destroyed). V(V), Hg2+, Ni2+, Cu2+ and Pd2+ can interfere. Determination of cobalt in cyanocobalamine and potable waters is possible in this way. Errors are between — 3 and — 7% (1.8–9 μg Co/l).
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    Fresenius' Zeitschrift für analytische Chemie 306 (1981), S. 401-401 
    ISSN: 1618-2650
    Keywords: Best. von Niob in Stahl ; Spektralphotometrie ; Sulfobenzolazodihydroxypyridin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 308 (1981), S. 431-433 
    ISSN: 1618-2650
    Keywords: Best. von Proteinen ; Spektralphotometrie ; Gegenwart von Dodecylsulfat und Mercaptoethanol, modif. Biuretmethode
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The biuret method was modified to tolerate the presence of 100 mg of SDS and 21 mg of ME in a sample volume of 500 μl. The modification concerns in particular the concentrations of copper sulphate and sodium citrate, an addition of propanol-2 for preventing precipitation of SDS and use of H2O2 for oxidizing ME. The determination of SDS-soluble proteins in starch-containing solutions is discussed.
    Notes: Zusammenfassung Eine Weiterentwicklung der „SDS-Biuretmethode“ [15] wird beschrieben. Die Modifikation betrifft hauptsächlich die Konzentrationen von Kupfersulfat und Natriumcitrat, einen Zusatz von Propanol-2 zur Verhinderung einer Fällung von SDS sowie die Verwendung von H2O2 zur Oxidation von ME. Die Methode toleriert bis zu 100 mg SDS und 21 mg ME im eingesetzten Probenvolumen (500 μl). Eine Möglichkeit zur Durchführung der Bestimmung in Gegenwart von Stärke wird beschrieben und diskutiert.
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  • 27
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    Fresenius' Zeitschrift für analytische Chemie 309 (1981), S. 400-400 
    ISSN: 1618-2650
    Keywords: Best. von Trichlorfluormethan in Luft ; Spektralphotometrie ; Pyridin
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    Fresenius' Zeitschrift für analytische Chemie 309 (1981), S. 373-376 
    ISSN: 1618-2650
    Keywords: Best. von Nickel ; Spektralphotometrie ; Verbesserung der Nachweisgrenze, Chromatographie
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Als Nachweisgrenze für das extraktiv-photometrische Bestimmungsverfahren von Nickel mit Pyridin-2-aldehyd-2-chinolylhydrazon (PAC) wurden als Absolutmenge 195 ng Ni ermittelt. Nach der dünnschicht-chromatographischen Abtrennung des PAC-Überschusses an Kieselgel mit Aceton kann die Nachweisgrenze auf 34 ng Ni verringert werden. Die Messungen erfolgen in Mikroküvetten in Benzol bei 515 nm; der Zeitbedarf für eine Bestimmung beträgt etwa 1 h. Die Techniken der Säulen- und Dünnschicht-Chromatographie (DC) werden miteinander verglichen; mit der DC ist der Zeitaufwand geringer. Es wird über die Analysenergebnisse in synthetischen Lösungen berichtet; eine Anwendung des Verfahrens z.B. für Nickel-Spurenanalysen in Lebensmitteln ist möglich, da das störende Eisen ebenfalls abgetrennt wird.
    Notes: Summary The determination limit in extractive spectrophotometric analysis of nickel with pyridine-2-aldehyde-2-quinolylhydrazone (PAC) was found to be 195 ng Ni (absolute amount of Ni). After separation of excess PAC by thin-layer chromatography on silicagel with acetone the determination limit can be lowered down to 34 ng. The measurements are carried out in microcuvettes in benzene at 515 nm, the time for one analyses being about 1 h. Column and thin-layer chromatographic techniques are compared; using TLC the necessary time is shorter. Results of analyses in synthetic solutions are discussed; an application of the procedure e.g. in Ni trace analysis in foodstuffs is possible, for interfering iron can be separated by TLC too.
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  • 29
    ISSN: 1618-2650
    Keywords: Best. von Rhenium ; Spektralphotometrie ; Thiocyanat u. Imipramin
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  • 30
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    Fresenius' Zeitschrift für analytische Chemie 309 (1981), S. 386-390 
    ISSN: 1618-2650
    Keywords: Best. von Formaldehyd ; Spektralphotometrie ; automatisiert
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Die photometrische Bestimmung von Formaldehydmit der Acetylaceton-Methodewurde automatisiert. Dazu wurden Bausteine der Flüssigkeits-Chromatographie verwendet. Der Zeitbedarf je Bestimmung beträgt 1–2 min, der Variationskoeffizient beträgt 0,1–0,2%. Je nach Ausführungsform können 0,1–200 mg/l Formaldehyd bestimmt werden.
    Notes: Summary The photometric determination of formaldehyde by means of the acetylacetone method is automated. For this purpose component parts of liquid chromatography are used. The time demand for one determination is 1–2 min, the variation coefficient is 0.1–0.2%. With two variations of the device concentrations from 0.1–200 mg/l formaldehyde can be determined.
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    Fresenius' Zeitschrift für analytische Chemie 309 (1981), S. 401-402 
    ISSN: 1618-2650
    Keywords: Best. von α-Ketoglutarsäure ; Spektralphotometrie ; Diaz. Aminobenzoesäure
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    Fresenius' Zeitschrift für analytische Chemie 305 (1981), S. 26-28 
    ISSN: 1618-2650
    Keywords: Best. von Wasser in organ. Lösungsmitteln ; Spektralphotometrie ; Pyridiniumphenolbetain, 2-Parameter-Gleichung
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Ein neues Verfahren zur Bestimmung von Wasser in organischen Lösungsmitteln (auch in Spuren) wird beschrieben. Die Solvatochromie des Pyridiniumphenolbetains E T30, die über eine einfach auszuführende UV-Absorptionsmessung bestimmt wird, ermöglicht zusammen mit einer zwei-Parameter-Gleichung eine exakte Wasserbestimmung in organischen Lösungsmitteln als Schnelltest und stellt damit eine Alternative zur Karl-Fischer-Titration dar.
    Notes: Summary A new procedure for the determination of water (even in trace amounts) in organic solvents is described. The solvatochromism of the pyridiniumphenol betaine, E T30, determined by a simple UV-absorption measurement, together with a two-parameter equation, permits an exact determination. The procedure is rapid and is, therefore, an alternative to the Karl-Fischer titration.
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  • 33
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    Fresenius' Zeitschrift für analytische Chemie 305 (1981), S. 287-288 
    ISSN: 1618-2650
    Keywords: Best. von Phosphorsäurephenylesterdiamid in Düngemitteln ; Spektralphotometrie ; neben Zusatzstoffen
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  • 34
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    Fresenius' Zeitschrift für analytische Chemie 305 (1981), S. 374-378 
    ISSN: 1618-2650
    Keywords: Best. von Thorium in Gesteinen, Zement, Wasser ; Spektralphotometrie ; Spuren, Extraktion mit Triphenylarsinoxid in Chloroform
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Thorium wird durch Extraktion mit Triphenylarsinoxid in CHCl3 und Rückextraktion mit 4 M HCl auf ein kleines Volumen konzentriert. Die Endbestimmung erfolgt spektralphotometrisch als Arsenazo-III-Komplex bei 660 nm in Mikroküvetten. Auf diese Weise konnte vor allem die Bestimmung von Spurenmengen Th wesentlich verbessert werden. 7 ng Th sind in bis zu 200 ml Ausgangslösung noch bestimmbar. Untersuchungen mit über 60 Kationen und etwa 20 Anionen zeigten, daß diese in weiten Grenzen nicht stören. U6+ wird zwar auch mitextrahiert, gibt aber in der salzsauren Rückextraktionslösung mit Arsenazo III einen etwa 15mal weniger lichtabsorbierenden Farbkomplex. Da aber Uran von den getesteten Kationen trotzdem am meisten stört und in Analysenproben das Th oft begleitet, werden weitere einfache Maßnahmen gezeigt, die einen bis zu ∼5000fachen Überschuß an Uran erlauben. Es wurde gefunden, daß auch die Seltenen Erden nicht stören und die zum Test verwendeten Seltenen Erd-Chemikalien Th enthalten. Bestimmungen in Standardgesteinen und Zementproben bestätigen die Anwendbarkeit der Methode.
    Notes: Summary Thorium is concentrated to a small volume by extraction with triphenylarsine oxide in chloroform and back extraction with 4M HCl. The spectrophotometric determination is then carried out in a micro cuvette using the absorption of the arsenazo III complex at 660 nm. By this procedure a sensitivity of 7 ng of Th in 200 ml solution can be achieved. About 60 cations and 20 anions were found not to cause interferences in a wide concentration range. The most disturbing element is U6+ which is coextracted, but leads to an arsenazo complex, which absorbs light at 660 nm about 15 times less than the Th complex. By simple measures, up to 5000 times higher U contents, as to Th, can be tolerated. Also the rare earths do not disturb the Th determination and it was found, that most rare earths chemicals, which were used for the tests, contained Th. The reliability of the method was confirmed by the analysis of standard rocks and by comparing the Th analyses of concrete samples with those obtained by neutron activation analysis.
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  • 35
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    Fresenius' Zeitschrift für analytische Chemie 306 (1981), S. 400-400 
    ISSN: 1618-2650
    Keywords: Best. von Kupfer(II) ; Spektralphotometrie ; Citrat, EDTA
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  • 36
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    Fresenius' Zeitschrift für analytische Chemie 307 (1981), S. 128-128 
    ISSN: 1618-2650
    Keywords: Best. von Molybdän(V) ; Spektralphotometrie ; Extraktion ; Thiocyanat ; Amidin
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  • 37
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    Fresenius' Zeitschrift für analytische Chemie 305 (1981), S. 410-410 
    ISSN: 1618-2650
    Keywords: Best. von Uran(VI) ; Spektralphotometrie ; Salicylaldimin-antipyrin
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  • 38
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    Fresenius' Zeitschrift für analytische Chemie 305 (1981), S. 415-416 
    ISSN: 1618-2650
    Keywords: Best. von Metol ; Spektralphotometrie ; Phenol, Sauerstoff
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  • 39
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    Fresenius' Zeitschrift für analytische Chemie 306 (1981), S. 32-32 
    ISSN: 1618-2650
    Keywords: Best. von Titan(IV) mit Lobelin ; Spektralphotometrie ; Thiocyanatkomplex
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  • 40
    ISSN: 1618-2650
    Keywords: Best. von Uran in Referenzmaterialien ; Spektralphotometrie ; Ionenaustausch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary A method is described for the highly accurate determination of trace amounts of uranium in standard reference materials. The uranium is separated from the bulk elements by anion-exchange chromatography, eluting most elements with 6 M hydrochloric acid and iron(III) with 0.5 M hydrochloric acid in 90% acetone. After elution of uranium with 0.1 M hydrochloric acid, residual traces of other elements are separated by a very selective cation-exchange procedure using a 3 g resin column. Finally the uranium is determined in the hexavalent state by spectrophotometry at 672 nm of its complex with chlorophosphonazo III at pH 1.1±0.2 in the presence of DTPA. Results are very accurate and precise even on a semi-routine basis. Relevant elution curves and results are presented for recovery tests and for the analysis of the 10 South African UREM standard materials.
    Notes: Zusammenfassung Das Uran wird von den Hauptelementen durch Anionenaustausch abgetrennt, wobei die meisten Elemente mit GM HCl und Eisen(III) mit 0,5 M HCl in 90 %igem Aceton eluiert werden. Nach der Elution von Uran mit 0,1 M HCl werden die restlichen Spuren anderer Elemente durch ein selektives Kationenaustauschverfahren (3 g Harz) abgetrennt. Das Uran wird schließlich in der sechswertigen Form als Chlorphosphonazo-III-Komplex in Gegenwart von DTPA bei 672 nm (pH 1,1±0,2) spektralphotometrisch bestimmt. Selbst bei halbroutinemäßiger Ausführung werden sehr genaue Resultate erhalten (Wiederfindung 99,7–100%). Analysenergebnisse für 10 Südafrikanische Standardmaterialien werden angegeben.
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    Fresenius' Zeitschrift für analytische Chemie 307 (1981), S. 194-196 
    ISSN: 1618-2650
    Keywords: Best. von Uran(VI) in Extrakten ; Spektralphotometrie ; PAN
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The Spectrophotometric method for the determination of uranium(VI) in trialkylamine extracts using 1-(2-pyridylazo)-2-naphthol (PAN) as a colorimetric reagent has been examined. The Job and Mole Ratio methods suggest that the coloured product is a 1∶1 complex of uranium and PAN. The method can be applied to cover the concentration range 0 to 5 g uranium per litre of extract. Sulphate interference is eliminated in the method by removal with calcium ions before colour development. Interferences from other ions likely to be present in the aqueous liquor appear to arise largely from inhibition of the uranium partition into the amine phase.
    Notes: Zusammenfassung Das Verfahren, bei dem ein Uran-PAN-Komplex der Zusammensetzung 1∶1 gebildet wird, kann für einen Konzentrationsbereich von 0 bis 5 g U pro l Extrakt eingesetzt werden. Eine Störung durch Sulfat wird durch dessen Entfernung mit Calciumionen vor der Farbentwicklung verhindert. Störungen durch andere Ionen werden hauptsächlich durch Beeinflussung der Uranextraktion hervorgerufen.
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    Fresenius' Zeitschrift für analytische Chemie 308 (1981), S. 32-32 
    ISSN: 1618-2650
    Keywords: Best. von EDTA in Harn ; Spektralphotometrie ; 4-Aminoantipyrin
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  • 43
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    Fresenius' Zeitschrift für analytische Chemie 307 (1981), S. 373-377 
    ISSN: 1618-2650
    Keywords: Best. von Phosphor in Phosphormineralien ; Spektralphotometrie ; Flow-injection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary Based on the flow injection principle and by using small sample volumes and splitting of the colorimeter output, a good reliable and reproducible method for the determination of P2O5 in phosphate rock covering the range of 0–40% on a routine basis was achieved. The system described is suitable for the routine analysis of P2O5 in the prepared phosphate rock samples at a rate of approximately 90 samples per hour with a coefficient of variation of better than 1%.
    Notes: Zusammenfassung Ein zuverlässiges und gut reproduzierbares Verfahren wurde ausgearbeitet, das routinemäßig für den Bereich von 0–40% geeignet ist und auf dem Flow-injection-Prinzip bei kleinen Probevolumina und Splitting des Colorimeter-Output beruht. Etwa 90 Proben können pro Stunde analysiert werden (Variationskoeffizient besser als 1%).
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  • 44
    ISSN: 1618-2650
    Keywords: Best. von Nifuroxim und Furazolidon nebeneinander ; Spektralphotometrie ; Orthogonal-funktionen
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The orthogonal function method has been applied to the simultaneous determination of nifuroxime and furazolidone in admixture without the need of preliminary separation. Two procedures are proposed. The first one involves measurement of a suitable solution of the mixture in the range from 309 nm to 359 nm with 10 nm intervals to determine nifuroxime, and in the range from 345 nm to 395 nm with 10 nm intervals to determine furazolidone. The second procedure involves determination of either components through measurement at the previously mentioned wavelength range while the absorbance of the partner component is measured at its λmax; correction of interference is carried out using an calculated absorbance ratio. Both methods were successfully applied to the analysis of market preparations and further application for routine analysis is recommended. Recoveries were in general between 97% and 102%.
    Notes: Zusammenfassung Durch Anwendung von Orthogonalfunktionen können Nifuroxim und Furazolidon in einem Gemisch nebeneinander ohne vorausgehende Trennung bestimmt werden. Zwei verschiedene Verfahren werden vorgeschlagen. Bei dem einen erfolgen die Messungen für Nifuroxim im Bereich von 309 bis 359 nm in Intervallen von 10 nm und für Furazolidon von 345 bis 395 ebenfalls im 10 nm-Abstand. Beim zweiten Verfahren wird einer der Bestandteile bei den genannten Wellenlängen gemessen, während die Extinktion des anderen Bestandteils beim Absorptions-maximum gemessen wird. Die Korrektur für die Störung erfolgt über das berechnete Extinktionsverhältnis. Beide Verfahren wurden erfolgreich bei Handelsprodukten angewendet und werden für Routinebestimmungen empfohlen. Wiederfindungsraten lagen im allgemeinen zwischen 97 und 102%.
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    Fresenius' Zeitschrift für analytische Chemie 308 (1981), S. 441-444 
    ISSN: 1618-2650
    Keywords: Analyse von binären Flüssigkeitsgemischen, Best. von Wasser in Organ. Lösungsmitteln ; Spektralphotometrie ; solvatochrome Farbstoffe
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Ein neues Verfahren zur Bestimmung der Zusammensetzung binärer Flüssigkeitsgemische mit Hilfe solvatochromer Farbstoffe wird beschrieben. Die Analyse erfolgt durch einfache UV/VIS-Absorptionsmessung und ist unter Verwendung einer Zwei-Parameter-Gleichung ein exakter Schnelltest.
    Notes: Summary A new procedure for the determination of the composition of binary liquid mixtures by the use of solvatochromic dyes is described. The analysis, which consists of a simple UV/VIS absorption measurement in combination with a two parameter equation, provides an exact and rapid test.
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