Atomic emission spectrochemical analysis of human tissues

A procedure is developed for atomic emission spectrochemical analysis of human organs. The spectra in partially incinerated tissue samples are excited in an ac electric arc and registered by a photodiode array MAES. The developed procedure was used to analyze samples of liver and kidney extracted from corps for the concentration of ten microelements, Fe, Mg, Mn, Cu, Mo, Pb, Ni, Cd, Sn, and Ag. The mean arithmetical values and concentration ranges for these elements in 14 samples were calculated. The presented data are compared with the published ones for other regions over the world.     

Recent advances in instrumentation for absolute emission quantum yield measurements

The fluorescence and phosphorescence quantum yields (Φ) of standard solutions have been re-evaluated based on an absolute method using an integrating sphere equipped with a multichannel spectrometer. We have examined in detail the Φ value of ruthenium(II) tris(2,2′-bipyridine) complex which have been often used as the standards in the determination of quantum yields of transition-metal complexes. This revealed that the Φ values for [Ru(bpy)₃]²⁺ were 0.063 in deaerated H₂O, 0.040 in aerated H₂O, 0.095 in deaerated CH₃CN, and 0.018 in aerated CH₃CN, respectively, which are significantly higher than the previously accepted values.We have also examined the technical aspects in the determination of absolute emission quantum yields for lanthanide complexes and those of organic crystals of anthracene. For the accurate determination for lanthanide complexes, special care must be taken in the spectroscopic measurements because of their narrow absorption and emission bands. For organic crystals, the fluorescence quantum yields are reduced due to reabsorption, chemical impurities and structural defects. Our observations for highly purified anthracene crystals revealed that the lower limit value of Φ was 0.64.     

Atomic emission spectroscopy for the on-line monitoring of incineration processes

A diagnostic measurement system based on atomic emission spectroscopy has been developed for the purpose of on-line monitoring of hazardous elements in industrial combustion gases. The aim was to construct a setup with a high durability for rough and variable experimental conditions, e.g. a strongly fluctuating gas composition, a high gas temperature and the presence of fly ash and corrosive effluents. Since the setup is primarily intended for the analysis of combustion gases with extremely high concentrations of pollutants, not much effort has been made to achieve low detection limits. It was found that an inductively coupled argon plasma was too sensitive to molecular gas introduction. Therefore, a microwave induced plasma torch, compromising both the demands of a high durability and an effective evaporation and excitation of the analyte was used as excitation source. The analysis system has been installed at an industrial hazardous waste incinerator and successfully tested on combustion gases present above the incineration process. Abundant elements as zinc, lead and sodium could be easily monitored.     

Atomic emission spectrometry of metal oxides using shock tube excitation

The behavior of powdered samples in the region behind the incident and reflected shock wave were investigated. When the particle size is less than 8 μm, the powdered samples are effectively vaporized and excited to emit spectral lines. It was shown that the sample particles are scattered behind the incident wave and concentrated again in a narrow portion near the observation window by the use of a reflector so that intense emission can be attained. As an excitation source, the shock tube was used for the determination of trace metals contained in copper oxide.     

Atomic emission spectroscopy method for mixing studies in high power thermal plasmas

Atomic emission spectrometry was used to measure the distribution of concentration ratios and temperature in thermal plasmas produced by high power torches for process engineering. The spectroscopic method is based on absolute line intensity measurement and Abel inversion. Assuming local thermal equilibrium, the temperature is deduced from the absolute emission of an argon line and the concentration ratio is deduced from the emission ratio of two lines. Using the two dimensions of the camera for spatial and spectral resolution, fast measurements with high resolution can be done. The method has been tested on a 60 kW inductively coupled plasma torch at atmospheric pressure. The results show that the concentration ratios n(O)/n(Ar) and n(H)/n(Ar) can be measured with an accuracy of 25% and that errors due to deviations from LTE are small. Demixing occurs in the induction zone. The application of the method showed that hydrogen diffuses much more than oxygen. The main disadvantage of this method is that, using emission, it does not permit to measure the concentration in the “cold” zones in the center and at the edge of the plasma.     

Atomic emission analysis of human hair for the presence of trace elements

A procedure is developed for the atomic emission analysis of human hair with the preliminary acid mineralization of samples and excitation of spectra in samples of dry residues of hair mineralizate on the end face of a carbon electrode in an alternating current arch. Spectra were recorded on an MFS-8 spectrograph modernized with a MAES photodiode array. Using the developed analytical procedure, samples of hair were analyzed for the presence of Al, B, Ca, Cu, Mg, Mn, Fe, P, Pb, and Zn. The average concentrations and concentration ranges of these elements were calculated for samples collected from 42 donors. The results obtained were compared with the published data for other geographical regions.     

Atomic and molecular emission spectroscopy on an expanding argon/methane plasma

A supersonically expanding cascaded arc plasma in argon is analyzed axperimentally by emission spectroscopy. The thermal cascaded arc plasma is allowed to expand through a conically shaped nozzle in the arc anode into the vacuum vessel. In the nozzle monomers (C _n H _v ) are injected. The monomers are dissociated and ionized by the argon carrier plasma, and transported toward a substrate by means of the expansion. Emission spectroscopy is used to obtain temperatures and particle densities. By varying external parameters (e.g., arc power, gas flow rates) plasma parameters can be linked with (e.g. parameters (e.g., refractive index).     

Atomic fluorescence and atomic emission measurements with an image dissector echelle spectrometer

This paper deals with the investigation of an image dissector echelle spectrometer as an analytical instrument for flame atomic fluorescence spectrometry and for flame atomic emission spectroscopy. The fluorescence was induced by high-pressure xenon arc lamps, which emitted continuum spectra and had higher power ratings, i.e. 1.6 and 2.5 kW, than those normally used for the same purpose. The experimental set-up included two different types of premix burners and one type of total consumption burner. A spherical reflector was applied to improve the utilization of the fluorescence radiation. Two different coatings were tested. None gave the expected enhancement.Detection limits and growth curves were measured for 8 different elements (Ca, Co, Cu, Fe, K, Mg, Na and Ni) in a non-separated air/acetylene flame. The attained detection limits were found to be equally good or somewhat better in flame atomic fluorescence excited with continuum sources than previously reported in the literature, i.e. using similar flames. In flame atomic emission spectroscopy better detection limits have been reported before.     

Atomic emission of anhydrous hydrogen bromide: Spectra from 200 to 900 nm by sealed inductively coupled plasma-atomic emission spectroscopy

Anhydrous hydrogen bromide, at concentrations of up to 25%, has been introduced into a sealed inductively coupled plasma system for spectrochemical analysis. The emission spectra of 15% anhydrous hydrogen bromide is reported over the spectral range of 200 to 900 nm from an enclosed inductively coupled plasma discharge operated at atmospheric pressure and 1.1 kW. More than 140 atomic Br I lines are identified and reported along with their relative intensities. Where possible, molecular band assignments of Br₂ are made. Impurities identified qualitatively include Fe, Sn, C, and Ni. The presence of these impurities were verified by gas phase hydrolysis and subsequent inductively coupled plasma-mass spectrometry analysis.     

High-frequency instrumentation

The present work was undertaken to overcome the disadvantage of the limited concentration range of high-frequency measurements. Instruments which respond to either effective capacitance or effective conductance changes were used. A cell was designed to minimize the dielectric constant contribution of the solution, and respond only to conductance. Studies on the significance of the physical dimensions of high-frequency titration cells were carried out. Progressively varying the electrode separation distance or the diameter of the titration vessel shifted the useful concentration regions of the response curves. Increasing the length of the metal electrodes or decreasing the cell wall thickness magnified the response of the effective concentration regions. An equation was derived relating the specific conductance of the sample solution to the physical dimensions of the high-frequency cell necessary for maximum sensitivity. Constant-temperature systems were devised to permit both aqueous and non-aqueous liquids to be used as circulating media.     

Atomic emission and atomic absorption spectrometric analysis of high-purity powders for the production of ceramics

Summary Direct analysis methods and multistage combined analytical procedures for the determination of impurities at the g/g level and the upper ng/g level in high-purity powders of Al₂O₃, AlN, Si₃N₄ and SiC are described. Results obtained with a novel direct slurry-atomization technique using a Babington nebulizer and inductively coupled plasma optical emission spectrometry (ICP-OES) are presented. A comparison of analysis results of combined analytical procedures including wet chemical decomposition and determinations with graphite furnace atomic absorption spectrometry (ETAAS) or ICP-OES with those of slurry-atomization ICP-OES show the capabilities of this technique for routine analysis in production control. Detection limits for Al, B, Ca, Co, Cu, Fe, Mg, Mn, Si, Ti, W, V, and Zn in the matrices mentioned are between 0.03 and 2.5 g/g. For elemental concentrations 10 g/g relative standard deviations of the measurements are generally below 10%. The technique is shown to be a powerful tool for trace determinations in powder samples. This is shown by its use for analysis of a series of the ceramic powders mentioned and comparative results of other direct techniques such as total reflection X-ray fluorescence spectrometry and instrumental neutron activation analysis.

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OES und AAS von hochreinen Pulvern für die Keramikherstellung

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Herrn Prof. Dr. G. Tölg zum 60. Geburtstag von seinen Mitarbeitern gewidmet