Determination of chromium on metal surfaces by prompt proton spectrometry

Surface concentrations of chromium were determined non-destructively on copper and nickel substrates by prompt proton spectrometry during irradiation with 3.5 MeV deuterons. Ground state protons from⁵²Cr were used as a measure of the chromium content. The analysis required 5 to 30 min. The relative precision obtained was ±1.8% on copper and ±2.4% on nickel substrates, respectively.     

Contribution of activation analysis with low energy charged particles to studies on GaAs

It is shown that the instrumental analysis of carbon and oxygen in GaAs, at trace level, can be achieved by irradiation with low energy deuterons and tritons (3 MeV). The experimental sensitivities are 6 ppb/weight for the¹⁶O( ₁ ³ H,n)¹⁸F reaction and 25 ppb/weight for the¹²C( ₁ ² H,n)¹³N reaction. Applications related to the metallurgy of GaAs are described.     

Alpha activation of calcium and its possible use for analysis

This method is based upon the measurement of 3.95-hr⁴³Sc which is formed during α-activation from⁴⁰Ca, the most abundant (96.8%) isotope of calcium. The excitation function for the⁴⁰Ca(α, p)⁴³Sc reaction was determined and the maximum yield of⁴³Sc (about 10⁷ cpm per mg of calcium for a 1-hr irradiation at a beam current of 1 μA) was obtained at an irradiation energy of 14 MeV. The interference free sensitivity of the method at this energy was found to be 8.5·10^?12 g, for a 1-hr irradiation at a beam current of 10 μA. The elements most likely to interfere with the determination are potassium and scandium. The extent of this interference was investigated as a function of irradiation energy and methods to eliminate or subtract the activity formed from these elements are discussed. An attempt was made to determine non-destructively the calcium content of very pure silicon and aluminium and upper limits for the concentration of calcium in these samples were set at 0.27 ppb and 6.9 ppb, respectively. Magnesium, thulium oxide and yttrium oxide samples of known calcium content were also analysed.     

Determination of residual impurities in InP grown by the Czochralski method,using charged particle activation analysis

InP samples were analyzed by charged particle activation analysis. Proton activation at 12 MeV permits the nondestructive survey of 30 elements. The main impurities are Ti, Fe, Ga and Zn (10¹⁵ to 2·10¹⁶ at/cm³). Oxygen was analyzed separately by triton activation at 3 MeV; the oxygen concentration is normally less than 10¹⁶ at/cm³.     

Gold bearing ore assays using 197Au(γ,n)196Au photonuclear reaction

We performed computational and experimental studies of the feasibility of the gold bearing ore assay utilizing the ¹⁹⁷Au(γ,n)¹⁹⁶Au photonuclear reaction. Gold bearing silicate samples were irradiated using bremsstrahlung produced by an electron accelerator with endpoint energies ranging from 25 to 40 MeV. ¹⁹⁶Au yield simulations were benchmarked and experimental results were in good agreement with the predictions. Optimum electron beam energy for photon activation analysis was found to be around 32 MeV which corresponded to a detection limit of 80 ppb. Two-hour gamma-spectroscopy measurements were repeated every 24 h and the optimum sample cooling time was found to be about 100–160 h.     

Analyse multielementaire instrumentale des phosphates marocains par photoactivation nucleaire

Photonuclear activation and high resolution gamma-ray spectrometry have been used to determine non-destructively the concentrations of 25 trace elements in Maroccan phosphate rock. The activation was simultaneously performed for phosphate samples and multielement standards in the bremsstrahlung beam of a linear electron accelerator at 18 and 30 MeV maximum energies. Gamma-ray spectra were recorded with a 79 cm³ Ge(Li) detector and a programmable analyzer IN 96. A detailed study of interferences was carried out. Limits of detection between 0.5 and 125 μg·g^?1 were obtained.     

Use of a carboxylate exchanger in the determination of copper in distilled water by neutron activation analysis

Copper in distilled water is collected on Zeokarb 226(NH ₄ ⁺ ) and irradiated with thermal neutrons. By comparison of the induced activity of 0.51 MeV photopeak of⁶⁴Cu with that of a standard, irradiated under comparable conditions, copper at ppb levels is easily determined.     

Die Bestimmung von Submikromengen Kupfer in Reinstmetallen und Meteoriten Durch Ein Hochselektives γ,γ-Koinzidenzverfahren

Copper was determined non-destructively by neutron-activation analysis in the high purity metals Be, Bi, Pb, Se, Sn, Tl and in iron meteorite specimens down to concentrations of 40 ppb, while the minimum detectable mass for 1 g-samples as defined recently byCurrie ²⁵ was about 0.1 ppb Cu. γ,γ-coincidence counting of the annihilation radiation of⁶⁴Cu essentially improved suppression of interferences by other γ-cascade emitters. The latter was achieved by increasing the detector distances and by counting in centric and eccentric positions with respect to the detectors. Using the 180°-angle correlation of the annihilation γ-quants of⁶⁴Cu etc. an increase in selectivity—in relation to conventional coincidence methods—was achieved by a factor of about 10³. A goniometer arrangement proved to be very advantageous.      

External proton beam analysis of layered objects

Ion-beam analysis for determining the elemental composition and to obtain depth information has been carried out with MeV protons in air by means of simultaneous external PIXE and RBS. Stainless steel products of extended size and a historic painting are analyzed non-destructively. These objects include systems of layers with areal densities up to some ten mg/cm². Depth information is obtained by PIXE using energy variation of the primary proton beam and in addition directly from RBS for the outermost near-surface region. Main and secondary elements as well as impurities can be determined together with areal densities. Particularly, the knowledge on the depth distribution of the pigments in paintings provides information on paint techniques.     

Non-destructive profiling of fluorine in teeth to large depths

A new method for non-destructive depth profiling of fluorine has been developed which extends the profiling range to much larger depths than hitherto possible. In this method the thick-target yield of 6–7 MeV gammas from the reaction of ¹⁹F(p,αγ) ¹⁶O in the tooth sample, was measured as a function of the incident energy from threshold to up to 2.7 MeV and the yield curve plotted. This curve was compared to the calculated yield curve of 6–7 MeV gammas from the same reaction but on an enamel matrix containing uniformly distributed fluorine. The difference in the shape of the two curves was only due to the non-uniform distribution of fluorine in the tooth sample, which could then be calculated. By making use of this method F-depth profiles in teeth of monkeys were determined non-destructively to a depth of 14 μm. This method is also applicable for profiling other elements through appropriate resonant or non-resonant nuclear reactions.     

The determination of calcium in yttrium oxide by alpha-particle activation analysis

The determination of calcium in yttrium oxide through the⁴⁰Ca(α, p)⁴³Sc reaction was studied, using a post-irradiation radiochemical separation procedure. The half-life of⁴³Sc was determined to be 3.87 hr. The chemical recovery was about 70%. The detection limit was about 10 ppb, for a 30 min irradiation at an alpha-particle beam current of 1 μA (E_α=13.4 MeV) and γ−γ coincidence counting (background counts being<1, cpm), with counting starting at 4 hours after the end of irradiation. Four samples of a batch of yttrium oxide (A.R.) were analyzed, and found to contain 13.9±1.0 ppm of calcium.     

Voltammetric behavior and trace determination of Pb at a mercury-free screen-printed silver electrode

Screen-printed silver electrodes (AgSPEs), without chemical modification, has been investigated as disposable sensors for the measurement of trace levels of Pb²⁺. Potential segment analysis indicates that the formation of underpotential and bulk depositions of Pb is not strongly coupled on the AgSPE. The possibility of determining Pb²⁺ at trace levels using the reversible underpotential deposition peak was examined by square-wave anodic stripping voltammetry without removal of oxygen. Under the optimized analytical conditions, the obtained sensitivity, linearity, and detection limit are 0.355 μA/ppb, 5-80 ppb (r=0.9992), and 0.46 ppb (S/N=3), respectively. The electrode is quite stable for repetitive measurements. The interference effect was thoroughly studied with various metals and no significant change in current was found in the determination of 5 ppb Pb²⁺. The practical applications were demonstrated to measure trace Pb²⁺ in natural waters.     

Inkjet Printed Multi‐walled Carbon Nanotube Sensor for the Detection of Lead in Drinking Water

Electroanalytical methods can be used for the reliable detection of the toxic heavy metal lead in drinking water samples. Inkjet printed electrodes have potential for the rapid and affordable assessment of drinking water. Researchers have shown the electrochemical sensing applicability of inkjet printed electrodes. In this work, Pb²⁺ was detected using an inkjet printed multi‐walled carbon nanotube (IJP‐MW‐CNT) electrode with silver tracks printed underneath. The silver tracks provide the sensor with the conductivity needed for sensitive measurements. MW‐CNT were dispersed in water using bile salts as a surfactant to prepare the ink. The IJP‐MW‐CNT electrode was used as the working electrode with a platinum wire and Ag/AgCl as auxiliary and reference electrode, respectively. The electrodes performance was optimized in 0.1 M acetate buffer (pH=4.3) and had two linear ranges of 5 to 20 ppb (R²=0.99) with a sensitivity of 38 nA/ppb and 20 to 50 ppb (R²=0.98) with a sensitivity of 15 nA/ppb and a limit of detection (LOD) of 1.0 ppb for Pb²⁺. The analytical applicability of electrode was determined by constructing a calibration curve in an unaltered drinking water sample (i. e.) Cincinnati tap water with two linear ranges of 15 to 40 ppb (R²=0.99) with a sensitivity of 1.5 nA/ppb and 40 to 70 ppb (R²=0.99) with a sensitivity of 3.5 nA/ppb and a LOD of 1.0 ppb for Pb²⁺. Effects of copper and cadmium as potential interferents are reported.     

Studies in heavy ion activation analysis

¹⁵N induced radioactivation was used to study the possible trace determination of light elements with 1Z17. 55 nuclear reactions were investigated with ion beam energies ranging from E_1ab=10 MeV to E_1ab=30 MeV. Three elements were found to be determinable non-destructively, selectively and sensitively: Li, Be and Mg. Nuclear interferences have also been defined and quantified. The technique has been tested by analyzing NBS standards. Finally, Li and Be have been determined in glass samples and Mg in various types of alumina.     

On the determination of carbon and oxygen impurities in silicon by3He activation analysis

Carbon and oxygen impurities in silicon have been determined by 7.00 MeV³He activation analysis. The detection limits obtained for interference-free conditions are 0.1 ppb (wt) for carbon and 1.0 ppb (wt) for oxygen in silicon.     

Siloxane‐Crown Ether Polyamide Based Electrode for Electrochemical Determination of Lead(II) in Aqueous Solution

A siloxane‐crown ether polyamide copolymer (PDMS‐PA‐DB18C6) was electrochemically investigated for fabrication of lead‐sensitive electrodes for trace analysis in aqueous solutions. The PDMS‐PA‐DB18C6 electrodes were successfully evaluated for anodic stripping voltammetric determination of lead(II) as a promising alternative for the detection of lead at ppb levels. By a judicious choice of the deposition time, electrolyte concentration and pulse amplitude, good analytical performance of the developed sensor could be achieved, with a linear response in the range of 20–700 ppb, when LOD of 3.5 ppb could be attained. This method showed a good degree of selectivity and sensitivity for lead, suitable for the determination of Pb²⁺ in wastewater sample.     

Determination of sulfur in near-surface layers of materials by means of the32S(3He,p)34mCl nuclear reaction

The cross-sections of the³²S(³He, p)^34mCl nuclear reaction have been determined in the projectile energy region between 4.0 and 12.0 MeV with the aim of their use for the determination of sulfur in surface layers of materials by means of Charged Particle Activation Analysis (CPAA). The measured cross-sections indicate that the application of this reaction for the determination of ppm and sub-ppm concentrations of sulfur is possible depending on the matrix material (e.g. detection limit for S in GaAs is 2 ppm, whereas in Si 300 ppb).     

Trace determination of zirconium using charged particle activation

Reaction yields on thick zirconium targets with proton, deuteron,³He and⁴He activation have been measured and compared. The most favorable reaction combining high sensitivity and selectivity was found to be Zr(p, xn)⁹⁰Nb. The absolute cross-section for this excitation function has been measured for proton energies up to 20 MeV. Analytical applications are illustrated with nondestructive zirconium analyses in glass. Yields from the thick target experiments indicate that the detection limit for this zirconium analysis method is ～1 ppb.     

The problem of diffusion during charged particle activation analysis; the case of18F in pure germanium single crystals

During ion bombardment, thermal diffusion and radiation enhanced diffusion of atoms occur. These phenomena may be a source of error in ion beam analysis, particularly in radioactivation analysis if contaminant surface atoms are present. It is shown here that penetration of¹⁸F (derived from surface oxygen by nuclear reaction) in germanium single crystals, does not extend appreciably farther than the maximum range of the recoiling¹⁸F nuclei. Since the analyzed depth is over an order of magnitude larger than the recoil, the validity of charged particle activation analysis at the ppb level in the present case (oxygen→¹⁸F in germanium), is clearly demonstrated.