Direct analysis isotopes

Three common quantitative applications of radiochemical methods of analysis are considered in this section the direct analysis of radioactive isotopes by measuring their rate of disintegration, neutron activation, and the use of radioactive isotopes as tracers in isotope dilution. 

Direct Analysis of Radioactive Analytes The concentration of a long-lived radioactive isotope is essentially constant during the period of analysis. As shown in Example 13.6, the sample s activity can be used to calculate the number of radioactive particles that are present. 

The direct analysis of short-lived radioactive isotopes using the method outlined in Example 13.6 is less useful since it provides only a transient measure of the isotope s concentration. The concentration of the isotope at a particular moment... 

A logical approach which serves to minimise such uncertainties is the use of a number of distinctly different analytical methods for the determination of each analyte wherein none of the methods would be expected to suffer identical interferences. In this manner, any correspondence observed between the results of different methods implies that a reliable estimate of the true value for the analyte concentration in the sample has been obtained. To this end Sturgeon et al. [21] carried out the analysis of coastal seawater for the above elements using isotope dilution spark source mass spectrometry. GFA-AS, and ICP-ES following trace metal separation-preconcentration (using ion exchange and chelation-solvent extraction), and direct analysis by GFA-AS. These workers discuss analytical advantages inherent in such an approach. 

Isotopic analysis of amino acids containing natural abundance levels of 15N was performed by derivatization, GC separation, on-line combustion and direct analysis of the combustion products by isotope-ratio MS. The N2 gas showed RSD better than 0.1%c for samples larger than 400 pmol and better than 0.5%o for samples larger than 25 pmol. After on-column injection of 2 nmol of each amino acid and delivery of 20% of the combustion products to the mass spectrometer, accuracy was 0.04%e and RSD 0.23%o19. 

Sources of information about the isotopic composition of the upper portion of the lithospheric mantle come from the direct analysis of unaltered ultramafic xenoliths brought rapidly to the surface in explosive volcanic vents. Due to rapid transport, these peridotite nodules are in many cases chemically fresh and considered by most... 

A measure of the amount of a stable isotopic label that exceeds its natural abundance in unlabeled tracee. This is most directly accomplished using an ion ratio mass spectrometer to measure the ratio of ion currents for isotopomers such as C02 at mass 44 and 2 at mass 45. From the difference between the ion current ratio for a sample (Zsampie) and the ion current ratio for a reference gas (Zreference), the atom percent excess (APE) can be estimated. See Tracer/Tracee Ratio Compart-mental Analysis Isotope Exchange Kinetics... 

The introduction of inductively coupled plasma (ICP) in inorganic mass spectrometry means that there is an effective ion source operating at atmospheric pressure. Whereas solid mass spectrometric techniques allow direct analysis of solid samples in ICP-MS, the determination of trace impurities or isotope ratios in solid samples is often carried out after digestion and dissolution of the material. For the determination of trace impurities and isotope ratios in liquids, an additional nebulization... 

LA-ICP-MS is suitable for the direct analysis of materials such as metals, semiconductors, ceramics and insulators at trace and ultratrace levels (detection limits 1 ng g ) without sample preparation. The MS detection mode makes it possible isotope analysis and also isotope dilution methods using... 

For analysis of solutions, ICP-mass spectrometry (ICP-MS) is very promising (Houk et al., 1980 Houk, 1986 Bacon et al., 1990). Recent advances in separation and preconcentration techniques are discussed by Horvath et al. (1991). Bacon et al. (1990) report that although ICP-MS is a multi-element technique, recent papers tend to concentrate on a small number of target elements. With isotope dilution mass spectrometry (IDMS), detection limits are further reduced (Heumann, 1988) IDMS is also suitable for accurate speciation in very low concentration levels of elements (Heumann, 1990). For the direct analysis of solid samples, glow discharge mass spectrometry (GD-MS) (Harrison etal., 1986) is of interest. Tolg (1988) has suggested that a substantial improvement in the absolute detection power of GD-MS, as applied to micro analysis, can be expected, at least in comparison with the ICP as ion source. 

Leipziger, F. D., and W. J. Croft Geologic age determination by direct lead isotope analysis. Geochim. cosmochim. Acta 28, 268 (1964). 

The isotope dilution technique in LA-ICP-MS has been applied for the direct analysis of sulfur species in gas oil, diesel or heating fuel as described by Boulyga et al. In addition, these authors have developed an analytical method for the direct determination of halogens (Cl, Br and I) in powdered geological and environmental samples using isotope dilution laser ablation ICP-MS. The detection limits of LA-ICP-IDMS are in the low and sub-p,gg range for halogens. ... 

Orphan, V.J., House, C. H., Hinrichs, K. U., McKeegan, K. D., andDeLong, E. F. (2001). Methaneconsuming archaea revealed by directly coupled isotopic and phylogenetic analysis. Science 293, 484-487. 

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