Spectrophotometric methods for the determination of manganese

A comprehensive and critical review of the available spectrophotometric methods for the determination of manganese is presented. Details are given of a wide range of direct colour-forming reactions of manganese with organic ligands, which have been claimed to be of use in analysis for the metal. The use of the very sensitive kinetic methods of analysis is also discussed. It is found that there is a paucity of reliable detail concerning the general applicability of most methods to manganese determination and that there is even less detail on the comparative value of different methods for determination of the metal in particular types of matrix.     

Sequential determination of glucose and fructose in foods by flow-injection analysis with immobilized enzymes

A sequential method for determination of glucose and fructose involving the use of enzymes (hexokinase and glucose-6-phosphate dehydrogenase) immobilized on controlled-pore glass is proposed. The flow is selected so as to determine glucose or both sugars by fluorimetric determination of the NADH formed. The method is applied to the determination of these compounds in fruit juices, yoghourt and dessert powder with good results.     

Minimising the risk of some systematic errors by the use of the single vessel principle for cold vapour atomic absorption spectrometric determination of mercury in biological solids

The suitability of the single vessel principle (performing all steps of an analytical procedure in one vessel) for cold vapour atomic absorption spectrometric determination of mercury in biological solids was evaluated. The single vessel method gave a lower mean blank level with better precision, hence lower detection limits, as compared to the conventional method. The determination of total mercury in biological standard reference materials by the single vessel method also produced significantly higher mercury values and better precision than the conventional method. However, the mercury concentrations obtained in certified reference materials by the use of both methods were close to the mean certified values. Moreover, the use of the single vessel method is cost effective, rapid and environment friendly. The use of the single vessel technique is therefore recommended for accurate and reliable determination of mercury in biological solids.     

Determination of mercury by extraction and isotope-dilution mass spectrometry

The use of halides for determination of metals by stable-isotope mass spectrometry is suggested, and is illustrated by the use of mercury iodide for mercury determination.     

石墨炉原子吸收光谱法测定高温合金中镓

研究了普通石墨管、平台石墨管和涂钼普通石墨管对镓的测定性能.得出涂钼普通石墨管对镓的测定灵敏度和重现性均好于其他石墨管.从而建立了一种更为满意的石墨炉原子吸收测定高温合金中镓的新方法.     

Minimising the risk of some systematic errors by the use of the single vessel principle for cold vapour atomic absorption spectrometric determination of mercury in biological solids

The suitability of the single vessel principle (performing all steps of an analytical procedure in one vessel) for cold vapour atomic absorption spectrometric determination of mercury in biological solids was evaluated. The single vessel method gave a lower mean blank level with better precision, hence lower detection limits, as compared to the conventional method. The determination of total mercury in biological standard reference materials by the single vessel method also produced significantly higher mercury values and better precision than the conventional method. However, the mercury concentrations obtained in certified reference materials by the use of both methods were close to the mean certified values. Moreover, the use of the single vessel method is cost effective, rapid and environment friendly. The use of the single vessel technique is therefore recommended for accurate and reliable determination of mercury in biological solids. Received: 15 December 1997 / Revised: 9 April 1998 / Accepted: 18 April 1998     

Investigation of the use of thermometric titrimetry for the determination of acidic substances in wine

The use of thermometric titrimetry in the determination of acidic substances in red wine is described. The titration curve obtained in the thermometric titration of red wine with strong base presents two inflections. The stoichiometry corresponding to the first inflection presents good agreement with the so-called "total acidity" of wine, and is proposed for its determination. The second inflection is related to the content of phenolic substances in red wine.     

蔬菜水果中无机砷测定方法改进研究

研究改进了应用原子荧光法测定蔬菜水果中无机砷的前处理方法,用6 mol/L盐酸在70℃水浴中提取1 h,使试样充分浸提。吸取4 mL浸提液于10 mL容量瓶或具塞刻度试管中,加碘化钾-硫脲混合液1 mL,消泡剂(正辛醇)3~5滴,加水定容后测定试样中的无机砷。方法检出限为干样0.02 mg/kg,鲜样0.01 mg/kg,完全能够满足国家卫生标准限量和农产品认证指标测定的要求。     

Determination of aluminium-26 using a low-level liquid scintillation spectrometer.

The lack of a suitable tracer has severely limited the use of radioisotope tracer experiments in environmental and biological studies on aluminium. The only aluminium radioisotope with a half-life greater than 10 min is the long-lived positron emitter 26Al (t1/2 7.2 x 10(5) years). The exposure of this nuclide and the difficulty in attaining sufficiently low determination limits with standard radioanalytical techniques have restricted its application as a radioactive tracer. The development of a simple method for the routine determination of 26Al using Cerenkov counting and a Quantalus 1220 low-level liquid scintillation spectrometer is reported. For a 300 min counting time, determination limits of about 60 mBq in water samples and 120 mBq in biological (fish gill) samples can be attained. With these levels of determination, the use of 26Al as a tracer is a viable technique for the study of aluminium in environmental and biological systems.     

Simultaneous determination of acetaminophen and caffeine in tablet preparations by partial least-squares multivariate spectrophotometric calibration

The use of partial least-squares spectrophotometric calibration for the simultaneous determination of analgesic tablets in a multicomponent formulation is presented. This method is applied to the determination of acetaminophen and caffeine in tablet preparations. The results show that these components in a molar ratio of about 21:1 in tablets have been determined simultaneously with high precision.     

Sensitivity and detectability for manganese(II) determination in solution by kinetic methods of analysis

The use of nitrilotriacetic acid to enhance the catalytic effect of manganese ions on the oxidation of Malachite Green cations is reported. This effect permits a noticeable increase in sensitivity for the determination of micro and submicro amounts of manganese ions in aqueous solution. The detectability, however, is not so dramatically altered. Comparison is made with other kinetic methods for the determination of manganese in solution.     

Determination of phosphorus, sulfur and the halogens using high-temperature molecular absorption spectrometry in flames and furnaces—A review

The literature about the investigation of molecular spectra of phosphorus, sulfur and the halogens in flames and furnaces, and the use of these spectra for the determination of these non-metals has been reviewed. Most of the investigations were carried out using conventional atomic absorption spectrometers, and there were in essence two different approaches. In the first one, dual-channel spectrometers with a hydrogen or deuterium lamp were used, applying the two-line method for background correction; in the second one, a line source was used that emitted an atomic line, which overlapped with the molecular spectrum. The first approach had the advantage that any spectral interval could be accessed, but it was susceptible to spectral interference; the second one had the advantage that the conventional background correction systems could be used to minimize spectral interferences, but had the problem that an atomic line had to be found, which was overlapping sufficiently well with the maximum of the molecular absorption spectrum. More recently a variety of molecular absorption spectra were investigated using a low-resolution polychromator with a CCD array detector, but no attempt was made to use this approach for quantitative determination of non-metals. The recent introduction and commercial availability of high-resolution continuum source atomic absorption spectrometers is offering completely new possibilities for molecular absorption spectrometry and its use for the determination of non-metals. The use of a high-intensity continuum source together with a high-resolution spectrometer and a CCD array detector makes possible selecting the optimum wavelength for the determination and to exclude most spectral interferences.     

Spectrofluorimetric and isotachophoretic determination of maprotiline in human blood serum

Maprotiline determination in blood serum samples was investigated by the use of both capillary isotachophoresis and spectrofluorimetric techniques. The analyte had to be enriched before determination and extraction with n-heptane was used for this purpose. The preliminary separation enabled the determination of maprotiline in blood serum at therapeutic concentration levels.     

Selectivity of catalytic methods of determination

By means of catalytic analytical methods, extremely low levels can be determined at low cost and with a high sensitivity that is equal to that of physical methods of trace analysis. The selectivity of the catalytic determinations, is, however, usually rather lower than that of other methods of trace analysis. The selectivity can sometimes be improved by modification of the indicator reaction through variation of the reagents and their concentrations, or by use of masking reagents or activators, or by combination with a separation method. Modification of the indicator reaction can be exemplified by the selective determination of osmium and ruthenium by their catalysis of the nitrate oxidation of 1-naphthylamine. By variation of the nitrate concentration and the use of 1,10-phenanthroline and 8-hydroxyquinoline as complexing agents it is possible to determine these two elements simultaneously. An especially significant increase in the selectivity is made possible by use of a preliminary separation step. If the ion to be determined is separated by solvent extraction and then catalytically determined directly in the extract, a very specific determination is possible; this technique has been called "extractive catalytic determination". This method has been used for determination of molybdenum (0.5 ng/ml) in sea-water, iron (5 ng/ml) in heavy metal salts, and copper (3 ng/ml) in the presence of numerous elements.     

The use of ethylenediaminetetraacetic acid or nitrilo-triacetic acid as masking agents in the determination of palladium with dimethylglyoxime or quinaldic acid

The use of complexing agents to mask interference in the gravimetric determination of palladium has been studied. Ethylenediaminetetraacctic acid was used to complex interfering ions in the determination of palladium with dimethylglyoxime, and nitrilotriacetic acid has been employed as a masking agent in the determination of palladium with quinaldic acid. From 15 to 150 mg of palladium were determined. All the metals tested do not interfere with the exception of gold which s reduced by the complexing agents and has to be removed prior to the determination. The procedures are rapid, simple and accurate.     

Methods for the determination of adenosine triphosphate and other adenine nucleotides

The following methods for the determination of adenosine triphosphate reported in the past 25 years are considered: bioluminescence methods with the use of the firefly luciferase enzyme (with sensitivity to 10^?14 M); chromatographic methods (ion-exchange, thin-layer, and high performance liquid chromatography) for the determination of adenine nucleotides in mixtures with other nucleotides, nucleosides, and nitrogen bases; and fluorescence, spectrophotometric, and electrochemical techniques (including those with the use of sensors), which are promising but not commonly used for the determination of adenine nucleotides. The advantages and disadvantages of these methods are demonstrated.     

Flow injection determination methods of ascorbic acid

A review with 100 references is presented to show the advantages involved in the use of flow injection analysis (FIA) for the determination of ascorbic acid. The FI methods proposed for the determination of ascorbic acid are described and compared according to the used detection technique. Analytical figures of merit and interferences are also discussed.     

Selective Liquid and (Vinyl-Chloride) Pentoxyverine Membrane Electrodes - Their Preparation and Use for the Potentiometric Determination of Pentoxyverine Citrate

Abstract

The use of liquid and poly(vinyl-chloride) membrane electrodes which are sensitive and reasonably selective for pentoxyverine determination is described here. The electrodes are based on the use of pentoxyverine-picrate, pentoxyverine-picrolonate and pentoxyverine-tetraphenylborate ion association complexes as electroactive materials in nitrobenzene or in poly(vinyl chloride) matrix. These electrodes show near Nernstian response values in different concentration ranges, depending on the nature of the used counter-ions, at 3.3–7.8 pH range. Potentiometric determination of pentoxyverine citrate with use of these electrodes gives good results which later on are compared with those obtained by non-aqueous titration.     

Hydrogenation enthalpimetry--I: microcomputer-assisted calibration and data-acquisition

A calorimetric device is described which permits enthalpimetric determination of unsaturated hydrocarbons through the enthalpy change for their catalytic hydrogenation. Samples with weights from < 1 to about 20 mg can be analysed with a mean error of about 2%. The method makes extensive use of digital electronics and is well suited to routine automated determination of unsaturation. The principal drawback is lack of specificity.