Isotopic analysis of lithium by prompt alpha measurement during deuteron irradiation

Charged particle spectrometry was used to determine the isotopic concentration of lithium in lithium fluoride targets irradiated with a deuteron beam of 4.0 MeV. Alpha particles emitted by the⁶Li(d, α)⁴He and⁷Li(d, α)⁵He reactions were used as a measure of⁶Li and⁷Li, respectively. From the⁶Li/⁷Li α-count ratio the isotopic concentration of⁶Li was determined for isotopic concentrations over the range 7.42 (natural) to about 30 atom%⁶Li, with a relative standard deviation of±4.1%. Alpha particles from the¹⁹F(d, α)¹⁷O reaction could also be measured as an internal standard, extending the measurements from natural to 100 atom%⁶Li and giving a relative standard deviation of ±1.9%. The effect of target thickness on the accuracy of the determinations was investigated.     

Determination of low dose concentration profiles in solids by means of (n,p) and (n, α) reactions

The isotopes³He,⁶Li,⁷Be and¹⁰B exhibit extremely large cross sections, between 1 and 48 kilobarn, for (n, p) or (n, α) reactions with thermal neutrons. Together with now available extracted thermal neutron fluxes of 10⁽ n·cm⁻²·sec⁻¹ or more, these reactions present a highly sensitive method of detecting the mentioned light elements in any heavy matrix material. Through the experimentally determined energy losses of the emitted protons or α-particles, also well resolved depth profiles can be obtained, as demonstrated here for some relevant examples from semiconductor and fusion technology.     

Determination of lithium and its isotopic composition by activation analysis and measurement of8Li and17N

The non-destructive determination of lithium was performed by using a Cerenkov counter for the detection of the 13 MeV (max) β-particles from the 0.84 sec⁸Li produced by the reaction⁷Li(n,γ)⁸Li. Under optimal conditions for a favorable signal-to-noise ratio, a count rate of about 35 cps/μg lithium at the beginning of the measurement was obtained, with a background of 4.5 cps and a working range of 3–400 μg lithium. The interference of other elements was studied. Several lithium-containing minerals and a sample of Dead Sea water were analyzed. The isotopic composition of lithium in aqueous solutions was determined by the simultaneous measurement of the neutrons produced by the reactions⁶Li(n,α)t and¹⁸O(t,α)¹⁷N, and the β-particles emitted by⁸Li.     

Light element profiling using nuclear reaction analysis on tapered corrosion sections

A scanned microbeam has been used to profile tapered corrosion sections of thickness up to 500 μm. The method of beam scanning and data collection is described and selected profiles are presented for the reactions D(³He, p)α,¹²C(d, p)¹³C,¹⁴N(p, α)¹²C and¹⁸O(p, α)¹⁵N. Finally the advantages and limitations of the technique are discussed.     

Search for molecular effects in range corrections: Lithium determination by proton bombardment

Three different proton-induced reactions were used to analyze 19 pure lithium compounds of known composition. Prompt alpha-particles were measured from the reaction⁷Li(p, )⁴He at E_p=4.5 MeV and prompt gamma-rays of 429 and 479 keV from the ractions⁷Li(p,n)⁷Be and⁷Li(p,p)⁷Li, respectively, at E_p=4.5 MeV. Elemental stopping powers were calculated from tables and used to compute the stopping power of the target matrices by Bragg's Law. Apparent discrepancies in the measured yield could point to deviations from Bragg's Law and hence to molecular effects. The maximum value for any molecular effect was found to be <5.5%.     

Determination des fonctions d'excitation des reactions19F(p, α0)16O et7Li(p, α0)4He entre 150 et 1800 keV

The experimental device used is described. Excitation functions are given for an angle of observation 150° with respect to the incident beam. The possibilities of applying these reactions to the measurement of surface lithium and fluorine concentrations are considered. The detection limits for these two elements are shown to be 5·10⁻³ μg·cm⁻² with protons of energy between 1,350 and 1,500 keV. The method is compared with that based on the detection of prompt γ-rays from the reactions⁷Li(p, γ)⁸Be and¹⁹F(p, α γ)¹⁶O.      

Comparison of the3He/16O and1H/18O prompt nuclear reactions for lattice location measurements of oxygen in niobium

Experimental data are presented for comparison of the determination of oxygen by the¹⁶O(³He, p)¹⁸F,¹⁶O(³He, α)¹⁵O and¹⁸O(p, α)¹⁵N prompt nuclear reactions, and of their use in the lattice location, by the ion-channelling technique, of oxygen atoms in single crystal targets of elements such as niobium, where oxygen contents of ≈0.1 atomic % or more can be obtained. Both reaction cross-sections and lattice-defect production rates are considered in the comparison. Details are given of an arrangement for automatic crystallographic angular scanning of nuclear reaction and backscattering yields in channelling/lattice location measurements.     

Determination of isotopic composition of lithium by neutron activation analysis; comparison with mass spectrometry

An activation analysis method is described for routine determination of⁶Li-abundances in various lithium compounds on the basis of the reaction sequence⁶Li(n,α)T and¹⁶O(t, n)¹⁸F and the measurement of¹⁸F. Irradiations of diluted equeous solutions of samples containing CrO₃ as internal flux monitor were carried out at a thermal neutron flux density of ϕ≤10¹¹ n·cm⁻²·sec⁻¹. Interferences from variations in neutron self-shielding oxygen concentration and triton range do not exceed 0.5% when using the dilution technique. The results for⁶Li abundances from 3.52 to 7.60% with standard deviations of 1 to 2.5% were confirmed by mass spectrometric measurements.     

Yields and average cross sections of recoil charged particle induced reactions on11B,12C,13C,14N,16O and18O

The yield and average cross section for the reactions¹¹B(p, n)¹¹C,¹²C(p, )¹³N,¹³C(p, n)¹³N, ₁₂ ¹² C(d, n)¹³N,¹⁴N(p, )¹¹C,¹⁶O(p, )¹³N,¹⁶O(d, n)¹⁷F,¹⁶O(t, n)¹⁸F, and¹⁸O(p, n)¹⁸F have been measured in different compounds. The charged particles were created in the samples themselves either through recoil by scattering of 14 MeV neutrons off hydrogen and deuterium, or by the (n, t) reaction on⁶Li using thermal neutrons. The yields of reactions¹²C(d, n);¹⁶O(p, );¹⁶O(t, n) and¹⁸O(p, n) have been measured using proton, deuteron and triton spectra generated by 14 MeV neutrons in the reactions D(n, p)2n;⁶Li(n, d);⁷Li(n, d) and¹⁰B(n, d);⁷Li(n, t) and¹⁰B(n, t), respectively.     

Detection of stable isotopes with A (n, α) nuclear reaction: Application to the measurement of unidirectional fluxes of borate in a plant

The unidirectional influx of borate has been studied inLemna minor plants with the aid of purified boron isotopes,¹⁰B and¹¹B. Isotope¹⁰B was detected specifically by nuclear reaction¹⁰B(n, α)⁷Li in the presence of “homogeneous” detectors. Despite technical difficulties in performing the¹⁰B-estimations in the plant samples themselves, the results obtained here were consistent with those of efflux experiments, published previously, where the¹⁰B-measurements were performed in the external solution. Kinetic parameters of borate transports inLemna minor have been calculated.     

Preparation of manganese-53

The nuclide⁵³Mn was produced by the following three nuclear reactions,⁵²Cr(d, n)⁵³Mn,⁵¹V(³He n)⁵³Mn and⁵⁰Cr(α, n), (α, p)⁵³Mn. Enriched⁵²Cr and⁵⁰Cr metal targets were prepared on copper plate holder by electrodeposition. The commercially available natural vanadium foil was used for the⁵¹V(³He, n)⁵³Mn reaction. Each target was bombarded in a cyclotron. Manganese was extracted and purified without using carrier from the bombarded targets by anion and cation exchanges and solvent extraction. The isotopic ratio⁵³Mn/⁵⁵Mn was measured by mass spectrometry and the amount of⁵⁵Mn was determined by neutron activation analysis. The activity of⁵³Mn obtained was 7 dpm by 750 millicoulombs in³He bombardment (E³He=20 MeV). The activity due to by-product⁵⁴Mn was about several thousands times higher than that of⁵³Mn in³He and deuteron bombardments, which were produced through⁵¹V(³He, γ)⁵⁴Mn and⁵³Cr(d, n)⁵⁴Mn. In alpha bombardment (E_α=15 MeV), the activity of⁵³Mn produced was 8 dpm by 95 millicoulombs. The activity ratio, dpm⁵⁴Mn/dpm⁵³Mn, was about 3, and this ratio was the best one among the results so far obtained.     

The development of nuclear microprobe techniques for the spatial determination of13C and13C/12C ratios

Sensitive and selective nuclear reaction methods have been sought for the nuclear microprobe measurement of the spatial distributions of¹³C and¹³C/¹²C ratios. The¹³C(α, n)¹⁶O reaction, with neutron detection, is the most selective for¹³C, and has a sensitivity of ca. 100 ppm. The reactions¹³C(d, p)¹⁴C and¹²C(d, p)¹³C, with proton detection, are the most sensitive for the simultaneous measurement of¹³C and¹²C, with detection limits of 30 and 2 ppm respectively. Less sensitive alternative reaction pairs are;¹³C(³He, p)¹⁵N and¹²C(³He, p)¹⁴N;¹³C(d, nγ)¹⁴N and¹²C(d, pγ)¹³C;¹³C(³He, pγ)¹⁵N and¹²C(³He, pγ)¹⁴N. The conditions governing their use, particularly light element interferences, are detailed.     

Determination of oxygen with reactor neutrons

Oxygen in silicon was determined by the secondary nuclear reactions of⁶Li(n, α)T and¹⁶O(t, n)¹⁸F. Lithium fluoride was deposited in vacuum on fused quartz, covered with the sample and irradiated in a nuclear reactor. The depth profiles of¹⁸F in fused quartz and in silicon were observed, and enough depth to eliminate surface oxygen was estimated. On the basis of these results, oxygen was determined by the average cross-section method. Oxygen concentration in CZ silicon with various growing condition was 5–26 ppm and was consistent with those determined by the infrared absorption method. The detection limit of oxygen in silicon is 5 ppm.     

Radiochemical methods in the determination of nuclear data for fusion reactor technology

Nuclear data needs for fusion reactor design are briefly outlined. A summary is given of the radiochemical methods like precipitation, co-precipitation, liquid-liquid extraction, ion-exchange and high-pressure liquid chromatography which have been applied in the determination of cross-section data for (n, p), (n, n' p), (n, α), (n, n′p), (n, α), (n, n′ α), (n, t) and (n³He) reactions at 14 MeV, especially on potential wall materials and transmuted species. The measured data are discussed briefly. A radiochemical method is described for the experimental determination of space dependent tritium production rate in a lithium model blanket. Tritium was separated from Li by vacuum extraction and was determined quantitatively by gas phase β⁻-counting. A comparison of the experimental and computational results is given.     

A comparative study of234U/238U alpha-activity ratios determined by alpha-spectrometry and calculated from mass spectrometric data

²³⁴U/²³⁸U α-activity ratios determined by α-spectrometry (AS) and those calculated from the atom ratio data using the half-life values are compared in some of the isotopic reference materials of uranium and a few other uranium samples. For α-spectrometry, electrodeposited sources were prepared and a large area passivated ion implanted (IPE) detector (450 mm²) was used for recording the α-spectra. The isotopic composition of U was determined by thermal ionisation mass spectrometry (TIMS) and the recommended half-life values of²³⁴U and²³⁸U were used to calculate the α-activity ratio. It is observed that²³⁴U/²³⁸U α-activity ratios calculated from the atom ratio data are consistently high, with a mean difference of about 5%, when compared to the α-spectrometry results. This discrepancy warrants confirmation by a few more laboratories and suggests redetermination of the half-life values of²³⁴U and²³⁸U.     

Determination of lithium and halogens and the significance of lithium to the understanding of cosmochemical processes

With a newly developed method fluorine and the other halogens have been measured in terrestrial, meteoritic and lunar samples. As a valuable byproduct lithium was determined also via teh reactions⁶Li (n,α)t→¹⁶O (t, n)¹⁸F. From our measurements the following new values for the “cosmic” abundance are derived (in atoms per 10⁶ Si atoms) F 750, Cl 4350, Br 8.83, and I 1.14. We could show that the Li/Be or Li/Zr ratios can be used to estimate the ratio of the Mg-silicates to the group of refractory elements and in course to calculate the bulk composition of the Moon and other planetary objects.     

Triterpene glycosides fromTupidanthus calyptratus I. Structure of glycosides B1, B2, F1, and F2 from leaves of hooded tupidanthus

Chromatographically inseparable mixtures of oleanolic and ursolic 3-O-α-L-rhamnopyranosyl-(1→2)-O-α-L-arabinopyranosides (glycosides B₁ and B₂) and their 28-O-α-L-rhamnopyranosyl-(1→4)-O-β-D-glucopyranosyl-(1→6)-O-β-D-glucopyranosyl esters (glycosides F₁ and F₂) are isolated from the leaves ofTupidanthus calyptratus Hook f. (Araliaceae). The structures of the isolated glycosides are established from chemical methods and¹H and¹³C NMR spectra. Glycoside F₂ is a new triterpene glycoside. Simferopol' State University. Translated from Khimiya Prirodnykh Soedinenii, No. 5, pp. 627–633, September–October, 1999.     

A compilation of charged particle production cross-sections by 14 MeV neutrons for Nb and Mo isotopes

A compilation of the cross sections (n, p), (n, n′ p), (n, α) (n, n′ α) and (n,³He) for⁹³Nb,^{92,95,96,97,98,100}Mo by 14 MeV neutrons is presented in the form of a table containing the results of nearly 70 different measurements, mainly obtained by activation analysis. Brief assessments of the experimental methods and the data status are given.     

Hydrogen and deuterium analysis by heavy ion activation

The use of heavy ion activation as a method for the analysis of hydrogen and deuterium has been evaluated. Thick target yields from reactions of⁷Li,¹⁰B,¹¹B and¹⁹F on¹H and²H have been determined; activation curves for many of these reactions are presented and interferences are evaluated. Hydrogen has been determined in titanium via¹H(¹⁰B, α)⁷Be at the 100 and 33 ppm levels with relative precisions of 8 to 10%.