On the determination of phosphorus via charged particle activation analysis

The application of charged particle activation analysis to the determination of phosphorus in a variety of sample materials is discussed. The activity produced via the³¹P(, n)^34mCl reaction is quantitated either nondestructively or using postirradiation radiochemical separations depending on the characteristics of the sample matrices. Corrections which are necessary for the determination of phosphorus in pure tantalum metal due to spectral interferences are discussed.     

On the determination of sulfur by charged particle activation analysis

An analytical method is described for the determination of trace amounts of sulfur by charged particle activation analysis. The method consists of proton irradiation followed by a rapid radiochemical separation of the product nuclide,^34m Cl. This procedure has been applied to a number of pure metal samples which range in sulfur content from 0.3 to 30 ppm. All analyses were repeated several times to ensure consistent results and to better evaluate experimental detection limits and systematic errors. The results indicate that sulfur determinations can be performed at a concentration of less than 1.0 ppm. Activation curves are presented for the reactions S(d,x)^34mCl, S(p,x)^34mCl, and the interfering reaction³⁵Cl(p, pn)^34mCl. In memoriam.     

Standardization in charged particle activation analysis

Standardization methods in activation analysis with charged particles are studied critically. Several approximate standardization methods that do not require knowledge of the excitation function are compared with the “numerical integration method” using excitation function data from the literature. It is shown that these methods yield accurate results if the threshold energy of the considered reaction is high and if sample and standard have a comparable Z value. A method that gives a rapid estimate of the maximum possible error is also presented. It is shown that for the “numerical integration method” the accuracy of the excitation function data has only a small influence on the overall accuracy. The influence of the accuracy of stopping power data and of possible deviations from Bragg's rule for light element standards is also considered. “Bevoegdverklaard navorser” of the NFWO.     

Some applications of activation analysis for the determination of trace impurities in semiconductor materials

Summary It is shown that activation analysis can be applied with good success for the determination of trace impurities in semiconductor material. The specificity and sensitivity together with a reasonable reproducibility are demonstrated. As an example, a survey of the determinations carried out with Ge, Se and Si matrices is given.

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Einige Anwendungen der Aktivierungsanalyse zur Bestimmung von Spurenverunreinigungen in Halbleiter-Materialien

Zusammenfassung Es wird gezeigt, daß die Aktivierungsanalyse mit gutem Erfolg zur Spurenbestimmung von Verunreinigungen in Halbleiter-Materialien herangezogen werden kann. Spezifität, Empfindlichkeit und Reproduzierbarkeit dieses Verfahrens werden diskutiert. Als Beispiel wird ein Überblick über die Bestimmung der Verunreinigungen in Germanium, Selen und Silicium gegeben.

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Communications given at the meeting Analytisce Probleme der Reindarstellung von Halbleitern 24–25 September 1986, Wiesbaden.     

Determination of rare earth elements by charged particle activation analysis in geological materials

The rare earth elements (REE), Pr, Sm, Eu, Gd, Ho, Er and Tm have been determined by charged particle activation analysis using 40 MeV a-particles through radiochemical approach. The radiochemical separation of REE as a group has been carried out from the bulk matrix. It has been shown from the theoretical computation that the products obtained from (a,xn) reactions (x = 1, 2, 3) are more suitable compared to those from (a,pyn) reactions (y = 0, 1, 2) due to the former having higher cross section (of the order of thousand millibarns).     

Neutron activation analysis of semiconductor materials

Two examples of the use of neutron activation analysis for the characterization of semiconductor materials are given. 23 elements were determined in ASTM silicon intercomparison samples. Most elements are below the detection limits, which vary between 0.009–300 ng/g. CdS/CdTe thin films have been characterized by determining the Cd, Te, Cl, I and In concentrations of dissolved films. Parallel determinations in different samples of films prepared under identical conditions agreed within 0–53% (average deviation 21%) for Cl, Cd, In and I in CdS and 1.6–22% (average 8.7%) for Cd and Te in CdS/CdTe, respectively. It was determined both by NAA and resonance ionization spectrometry (RIS). The order of magnitude of the results was 1 ng/g and they agree within the range 7–64% (average difference 25%). The analytical procedures are described and discussed.     

Routine charged particle activation analysis of light elements

In order to develop a highly reliable method of routine charged particle activation analysis on a commercial basis by request of an outside company, (1) a new target holder was developed for brittle or low melting-point samples, (2) some modifications and improvements were introduced in the chemical separation, and (3) the reliability of the results was further examined. Oxygen, nitrogen, carbon, and boron in a greater variety of matrices have thus become analyzable with a higher reliability and efficiency.     

Determination of trace elements in semiconductor materials by neutron activation analysis using the radioisotope addition technique

The determination of trace elements in highly activated matrix components was carried out by neutron activation analysis using the radioisotope addition technique. The method is based on the addition to the irradiated test sample of a radioisotope which is a diffeent nuclide of the element to be determined. After separation, the chemical yield is calculated from the radioactivity added and the element is determined by an ordinary technique. Twelve elements in indium phosphide and eight elements in gallium arsenide could be determined by the method.     

Secondary effects in prompt charged particle activation analysis

The phenomenon of secondary excitation was observed during irradiation of thick targets of boron and gallium nitride with 2 MeV³He⁺ ions. This effect, though negligible during irradiation with protons or⁴He⁺ ions, becomes significant when highly exoergic reactions can occur.     

Determination of oxygen impurity in high purity materials by charged particle activation analysis using alpha projectiles

40 MeV -particles have been used to determine oxygen impurity at ppm levels in silicon, copper, and stainless steel, through the radiochemical separation of¹⁸F from the matrix. The separation of¹⁸F has been carried out by two techniques, viz.(1) distillation of H₂SiF₆ and (2) precipitation of KBF₄ and some modification has been applied in the separation, depending on the nature of interferences from the matrix. Instrumental approach was also carried out to determine the oxygen impurity at 100 ppm in Si matrix because this approach is not possible in Cu and stainless steel samples due to matrix activity.     

The study of fundamental aspects of charged particle activation analysis

Two important problems are discussed: equations and data used for quantitation on one hand, diffusion under irradiation on another hand. It is suggested that recent semiempirical stopping power data for hydrogen and helium are sufficiently accurate to be used in any good calibration method, while for heavier ions it is preferable to use the “double reaction method”, which avoids the use of stopping power data. The problem of the additivity of the stopping powers in the case of compounds is also discussed and it is shown in a specific case that BRAGG-KLEEMAN's rule is valid. Deep diffusion under irradiation has sometimes been mentioned (e.g. F in Ge, Cu in Si): it can be an important source of errors in trace analysis. The possible deep diffusion of F in Ge has been studied: it is shown that such a diffusion does not occur, while surface contamination problems can lead to erroneous observations.     

Some problems of calibration technique in charged particle activation analysis

It is shown that three different approaches to calibration technique based on the use of average cross-section, equivalent target thickness and thick target yield are adequate. Using the concept of thick target yield, a convenient charged particle activation equation is obtained. The possibility of simultaneous determination of two elements impurities, from which the same isotope is formed, is pointed out. The calibration technique, in which thin standard is used but activation curve is not required, is discussed.     

A versatile charged particle activation technique for the analysis of the noble metals

The general usefulness of neutron activation analysis (NAA) for samples containing the platinum group elements (PGE) and Au, either as major or trace consituents, is discussed. Charged particle activation is shown to be a viable or complementary alternative. Proton (6–10 MeV) and alpha particle (9–15 MeV) beams, produced in a Tandem van de Graaff accelerater, have been established to be the most effective choice. By taking advantage of the Coulomb Barrier Effect and the fact that many charged particle induced reactions have relatively large threshold values, the same instrumental technique can be applied, with minor modifications, to a wide range of materials.     

A versatile charged particle activation technique for the analysis of the noble metals

The general usefulness of neutron activation analysis (NAA) for samples containing the platinum group elements (PGE) and Au, either as major or trace constituents, is discussed. Charged particle activation is shown to be a viable or complementary alternative. Proton (6–10 MeV) and alpha particle (9–15 MeV) beams, produced in a Tandem van de Graaff accelerator, have been established to be the most effective choice. By taking advantage of the Coulomb barrier effect and the fact that many charged particle induced reactions have relatively large threshold values, the same instrumental technique can be applied, with minor modifications, to a wide range of materials.     

An application of neutron activation analysis to biological materials

Contents of 13 trace elements in human hair were determined by neutron activation analysis. The distribution patterns of mean values of elements were extremely similar in all groups, though the contents of elements were individually different in each group. Numerous elements in new-born infants of both sexes correlated with each other, especially with V at a 95% confidence level. Special characteristics of diseased infants were the high contents of Cl and the low contents of Cr. It is presumed that these facts are due to the imbalanced acid-base equilibrium and some abnormal metabolic systems in diseased bodies.     

An application of neutron activation analysis to biological materials

Fourteen trace elements (short-lived nuclides: Al, Br, Cu, Mn and V; long-lived nuclides: Ag, Au, Cd, Co, Cr, Fe, Sc, Se and Zn) in human eye tissues are determined simultaneously by non-destructive neutron activation analysis. The quantity of Al, Br, Fe, Se and Zn in the eye tissues (about 1 to more than 10 μg/g dry weight tissue) seems to be higher than that of other trace elements, although content of each trace element in individual tissue are scattered in a wide range. Conjunctiva, iris (+ciliary body) and choroid (+pigment epithelium) seem to contain larger amount of various trace elements than other eye tissues. From correlation studies it is evident that the relative distribution of 14 trace elements in various eye tissues are similar, and furthermore the content of trace elements in the eye tissues may be correlated in each of the three groups (group A: Cd, Fe, Se and Zn; group B: Al, Cr, Fe, Se and V; group C: Al, Au, Fe and Se).     

Determination of boron in magnesium oxide by charged particle activation analysis

The determination of boron in magnesium oxide using the¹⁰B/p, /⁷Be,¹⁰B/d, n/⁷Be, and¹⁰B/d, n/¹¹C reactions is described. Lithium interferes the nuclear reactions leading to beryllium-7. Combination of a proton and deuteron irradiation, each followed by measurement of the induced beryllium-7 activity, allows a simultaneous determination of boron and lithium. The¹⁰B/d, n/¹¹C reaction is free from nuclear interferences. The boron concentration ranges from 1.5 to 850 g g^–1. The results obtained by the two methods are in good agreement.Senior Research Associate of the Belgian National Fund for Scientific Research.     

Charged particle activation analysis of phosphorus in biological materials

Charged particle activation analysis of phosphorus in biological materials using the³¹P (α,n)^34mCl reaction has been studied. Since^34mCl is also produced by the³²S (α,pn) and the³⁵Cl (α, α′ n) reactions, the thick-target yield curves on phosphorus, sulfur and chlorine were determined in order to choose the optimum irradiation conditions. As a result, it was found that the activation analysis for phosphorus without interferences from surfur and chlorine is possible by bombarding with less than 17 MeV alphas. The applicability of this method to biological samples was then examined by irradiating several standard reference materals. It was confirmed that phosphorus can readily be determined at the detection limit of 1 μg free from interferences due to the matrix elements.     

Application of the internal standard method coupled with the standard addition method in photon activation analysis to trace characterization of environmental materials

The internal standard method coupled with the standard addition method has been applied to the analysis of environmental materials, such as urban particulate matter, vehicle exhaust particulates and coal fly ash by photon activation. High-resolution gamma-ray spectrometry makes possible to use multi-internal standard gamma-rays, in order to crosscheck the analytical results obtained from each internal standard. It was ascertained that this method can provide not only accurate analytical results but also the information of homogeneity of samples, correlation of elements in the sample, loss or contamination in the preparation process.