Substoichiometric method in the simple radiometric analysis

The substoichiometric method is applied to simple radiometric analysis. Two methods-the standard reagent method and the standard sample method-are proposed. The validity of the principle of the methods is verified experimentally in the determination of silver by the precipitation method, or of zinc by the ion-exchange or solvent-extraction method. The proposed methods are simple and rapid compared with the conventional superstoichiometric method. The University has moved and changed its name and address as lollows: Institute of Chemistry, The University of Tsukuba 300-31 Sakura-mura, Ibaraki Japan.     

Applications of mass spectrometry in the trace element analysis of biological materials

The importance of mass spectrometry for the analysis of biological material is illustrated by reviewing the different mass spectrometric methods applied and describing some typical applications published recently. Though atomic absorption spectrometry is used in the majority of analyses of biological material, most mass spectrometric methods have been used to some extent for trace element determination in biomedical research. The relative importance of the different methods is estimated by reviewing recent research papers. It is striking that especially inductively coupled plasma mass spectrometry is increasingly being applied, partly because the method can be used on-line after chromatographic separation, in speciation studies. Mass spectrometric methods prove to offer unique possibilities in stable isotope tracer studies and for this purpose also experimentally demanding methods such as thermal ionization mass spectrometry and accelerator mass spectrometry are frequently used.     

Trace element analysis of biological materials by thermal and epithermal neutron activation analysis

A scheme for instrumental neutron activation analysis of biological materials is proposed. The scheme is based on a combination of thermal and epithermal activation. The accuracy is evaluated by analyzing 4 standard reference materials. Results from the analysis of human blood serum and plasma are given.     

Computer program for radiometric flow-injection analysis

Software for computer aided radiometric flow-injection analysis (CARFIA) was modified for working with a 386 AT Computer for data input from keyboard and for computing dispersion, concentration, peak height, constant k and S-half values.     

Application of nondestructive X-ray fluorescence analysis to determine the element composition of medicinal plants

A nondestructive X-ray fluorescence technique has been developed to determine Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, Ba, and Pb in plants. The line element intensities were measured by an S4 Pioneer X-ray sequence spectrometer (Bruker AXS, Germany). The inversely proportional relationship was obtained between the analyte line intensity and mass of the plant, pressed on boric acid backing, for elements with an atomic number 11 < Z < 20. It was found that reduction of plant mass from 6 to 1 g leads to an increase in element determination sensitivity. The detection limits for 1 g of pressed plant were evaluated as μg/g: 5–20 (Na, Mg, Al); 1–4 (Si, P, S, Cl, K, Ca, Ti, Ba, Pb); 0.4-0.8 (Cr, Mn, Fe, Ni, Br, Cu, Zn, Rb and Sr). This technique was applied to determine the element composition of violets of Violaceae family, which are used in medicine.     

Modified and reverse radiometric flow injection analysis

Determination of¹³⁷Cs and⁶⁰Co by using modified and reverse radiometric flow injection analysis is described. Two component RFIA was also realized using⁶⁰Co and¹³⁷Cs radionuclides.     

Application of neutron activation analysis for trace element determinations in biological materials

Over the past three decades, more and more interest has been focused on trace eleemnts in biological materials. This increasing interest has gone hand in hand with the continuous improvement of analytical techniques. Neutron activation analysis has proven to be a most suitable method for the quantitative determination of a wide variety of trace (0.01–100 μg g^?1) and ultratrace (<0.01 μg g^?1) elements in biological materials. This technique has even played a preponderant role in this field.     

Microwave assisted extraction for trace element analysis of plant materials by ICP-AES

Application of microwave assisted extraction for the decomposition and dissolution of plant samples for trace metal determination by ICP-AES was examined. Dried onion, leaves of spinach beet and three reference materials CTA-OTL-1, CTA-VTL-2 and CL-1 were analyzed. Water, EDTA and hydrochloric acid (0.01, 0.10 and 1.0 M, respectively) were used as leaching solutions. The extraction efficiency was investigated by comparison of the results with those obtained after microwave wet digestion. HCl was found to be very suitable for quantitative extraction of B, Ba, Cd, Cu, Mn, Ni, Pb, Sr and Zn from the samples. For reference materials, the measured concentrations are well consistent with the certified values. The use of EDTA led to a complete extraction of B, Cd, Ni, Pb, Sr and Zn. Water was found to be a good leaching solution for boron. For extraction with HCl and EDTA, the RSD values for the concentrations measured were below 8% for most of the elements.     

Enhanced trace element analysis of plant materials after accelerated pulsed UV digestion

A method for measuring trace concentration of Fe, Co, Ni, Cu, Zn and Pb in plant materials was developed, optimized, validated and compared using reference standards and fresh samples. The method is based on rapid material digestion by radicals produced with laser-assisted pulsed UV (PUV) photolysis of aqueous solutions containing H₂O₂. Metals in the resulting solution were pre-concentrated as carbamates. Samples were analyzed with particle induced X-ray emission (PIXE). Combined PUV digestion and pre-concentration techniques resulted in enhanced detection levels of selected trace elements in foods and non-food commodities. The method was applied to measure trace elements in wastewater irrigated fruits, vegetables and crops.     

Survey and evaluation of available biological reference materials for trace element analysis

Summary A database recently prepared by IAEA contains information on 60 internationally available biological reference materials (BRMs) from 9 producers. The data recorded for each material include: name, code No., cost, list of elements, and minimum weight of material recommended for analysis. For each element the concentration and its confidence interval (CI) are recorded, as well as an indication of whether the concentration value is certified or noncertified (e.g. an information value).Large differences among producers are observed in respect of how the concentration values and their CIs are defined, and how other relevant information is reported in the certificates of analysis. International recommendations on how this should be done generally do not seem to be followed.For several elements of biomedical interest there is a serious lack of BRMs namely: Al, F, I, Mo, Si, Sn and V. In addition, the CIs for the following elements are generally excessively large: Al, As, Cd, Cr, Hg, Mo, Ni, Se and V.     

Microwave assisted extraction for trace element analysis of plant materials by ICP-AES

Application of microwave assisted extraction for the decomposition and dissolution of plant samples for trace metal determination by ICP-AES was examined. Dried onion, leaves of spinach beet and three reference materials CTA-OTL-1, CTA-VTL-2 and CL-1 were analyzed. Water, EDTA and hydrochloric acid (0.01, 0.10 and 1.0 M, respectively) were used as leaching solutions. The extraction efficiency was investigated by comparison of the results with those obtained after microwave wet digestion. HCl was found to be very suitable for quantitative extraction of B, Ba, Cd, Cu, Mn, Ni, Pb, Sr and Zn from the samples. For reference materials, the measured concentrations are well consistent with the certified values. The use of EDTA led to a complete extraction of B, Cd, Ni, Pb, Sr and Zn. Water was found to be a good leaching solution for boron. For extraction with HCl and EDTA, the RSD values for the concentrations measured were below 8% for most of the elements. Received: 4 May 2000 / Revised: 20 June 2000 / Accepted: 22 June 2000     

Human hair analysis by PIXE: Pattern recognition of trace element composition

The feasibility is explored of classifying human hair specimens according to their trace metal composition as determined by PIXE. Protons of 3.5 MeV were used to analyse 150 samples by energy-dispersive spectrometry using a Si(Li) detector. The methods of the Minimal Spanning Tree and Non-Linear Mapping were used to establish correlation among the specimens. As a result of distinct groupings obtained by these methods it was inferred that these techniques could usefully be applied to environmental pollution studies.     

Development of nuclear and physical methods of element analysis of substance composition in the USSR

An up to date survey of recent trends in nuclear and physical methods developed in the USSR is given.     

Application of radiometric method for element migration determination from plastic packaging to food

In the present study, a radiometric method was applied for element migration determination from food plastic packaging to simulating solutions and foodstuffs. This method consisted of irradiating plastics with neutrons, its exposure for migration and radioactivity measurements in the food or food-simulating solutions. The migration was studied for water, juice, soft drinks, acidic fatty food and dairy product plastic packages. The results indicated Co, Cr and Sb migration to the simulating solutions and food. However, the contamination of these elements in food from packaging material was lower than the maximum limit values established by the Brazilian Surveillance Agency (ANVISA) legislation.     

An LC-ESI-MS method for the quantitative analysis of bile acids composition in fecal materials

In this work, a liquid chromatography coupled with electrospray ionization mass spectrometry (LC-ESI-MS) method was developed and validated for quantification of bile acids in fecal materials. Co-eluting matrix impurities in fecal materials have been shown to greatly suppress the ionization of analytes in mass spectrometry, which is known as the matrix effect. To correct large quantitative errors caused by the matrix effect, we developed a scheme that combined the standard addition method with internal standard (SA-IS). The fecal sample pretreatment involved a single step of extraction with ethanol. Bile acids were separated using a Luna C(18) column (150 mm, 2 mm i.d., 5 μm) with gradient elution. The deprotonated analytes were detected in selective ion monitoring mode. Our results showed that, by using this method, the accuracy of quantification was significantly improved in comparison to the conventional internal standard method. The linearity, sensitivity, accuracy and precision of the method were within the range of 0.05-5 μmol/L. This SA-IS method was successfully applied to the analysis of bile acids in the samples collected from patients diagnosed with inflammatory bowel disease.     

Multielement isotope dilution analysis by means of radiometric titration

A theoretical concept is derived for multielement isotope dilution analysis in a liquid-liquid extraction system. The practical performance is based on radiometric titration. To that purpose a prototype of a titration/extraction vessel with flow injection has been constructed. For calculations of the initial concentrations of the elements of interest from the experimental data, a computer program has been developed.     

Trace element analysis of archaeological materials and the use of pattern recognition methods to establish identity

Trace elements were determined in South West African potsherds by instrumental NAA and by PIXE. The elements for which the relative spread of concentrations were greatest were selected as indicators. From these the methods of the Minimal Spanning Tree and of Nonlinear Mapping were used to classify about 60 specimens. Groups were tested by concentration, sum of concentration and normalized concentration indices. Similar groupings were obtained irrespective of which analytical data or mathematical techniques was used.     

Development of caprine liver quality control materials for trace element analysis of biological tissues

Certified reference materials (CRMs) are used in analytical chemistry for method validation studies in order to establish measurement accuracy, traceability, and long-term stability throughout repeated analyses. Quality control (QC) during routine analysis requires access to stable materials appropriate for the sample matrix being analyzed. However, it may be difficult to find representative, low-cost QC materials, especially for specific analytes in biological tissue matrices. Here, four caprine liver pools are prepared for use as internal QC materials for trace element measurements in biological tissue. Analytes of interest include essential and nonessential trace elements and the lanthanide series elements. The suitability of caprine liver to serve as a secondary reference material (RM), as well as for routine QC purposes, is demonstrated through homogeneity and stability measurements, and the acquisition of precision and uncertainty data. Traceability is established for selected analytes for which available CRMs can provide an unbroken chain of calibrations.