The determination of boron in sedimentary rocks by neutron irradiation and prompt γ-ray spectrometry

Prompt γ-rays following the (n_th, α) reaction on¹⁰B have been measured to determine the boron content of sedimentary rocks. Employing an external reactor neutron beam with only modest flux, it is possible to assay boron at concentrations typically encountered in this material (>5 μg/g). The technique relies on the use of chemical standards and the values obtained for 9 North American shales are compared with measurements performed by emission spectrography. Detection limits and statistical errors as a function of beam time are also discussed. Department of Geology, Mcmaster University, Hamilton, Ontario (Canada)     

Determination of boron in materials by cold neutron prompt gamma-ray activation analysis

An instrument for cold neutron prompt gamma-ray activation analysis (PGAA), located at the NIST Center for Neutron Research (NCNR), has proven useful for the measurement of boron in a variety of materials. Neutrons, moderated by passage through liquid hydrogen at 20 K, pass through a (58)Ni coated guide to the PGAA station in the cold neutron guide hall of the NCNR. The thermal equivalent neutron fluence rate at the sample position is 9 x 10(8) cm(-2) s(-1). Prompt gamma rays are measured by a cadmium- and lead-shielded high-purity germanium detector. The instrument has been used to measure boron mass fractions in minerals, in NIST SRM 2175 (Refractory Alloy MP-35-N) for certification of boron, and most recently in semiconductor-grade silicon. The limit of detection for boron in many materials is <10 ng g(-1).     

Accurate and efficient determination of boron content in volcanic rocks by neutron induced prompt gamma-ray analysis

An accurate and efficient analytical method using neutron-induced prompt γ-ray was developed for the determination of boron contents in volcanic rocks. We corrected the effect of sample geometry and flux fluctuation by using silicon as an internal standard. However, we found that the slopes of the calibration line vary among volcanic samples with different matrix. Because the increase of boron activity correlates positively with γ-ray count rate of hydrogen (water), we call this as the hydrogen effect. The hydrogen effect was confirmed by our experiment in which the boron activities showed systematic increase with the amount of added hydrogen (water). Most volcanic rocks, however, contain little water (<2 wt.%) to show this effect. We determined boron contents in various volcanic rocks in order to confirm the validity of the procedure that we established. The analyzed boron contents agreed well with the previous reported values. For efficient PGA of boron in volcanic rocks, we recommend JB-2 (GSJ standard rock) as a single geochemical standard, because of its high boron content (31.2 ppm).     

Improvements in food analysis by thermal neutron capture prompt gamma-ray spectrometry

Summary The thermal neutron prompt gamma-ray activation analysis (PGAA) facility, operated by the US Food and Drug Administration and National Institute of Standards and Technology Center for Neutron Research, has been redesigned to lower background radiation levels and improved analytical capabilities. Analysis of 22 element standards and food and botanical certified reference materials revealed significant sensitivity increases and lower limits of detection for H, B, C, N, Na, Al, P, S, Cl, K, Ca, Fe, and Cd. Mass fractions for these elements, as well as Mg, Al, Si, Ti, Mn, Fe, Cu, I, Zn, Sm, and Gd, were determined for 6 dietary supplements.     

Determination of boron in borosilicate glasses by neutron capture prompt gamma-ray activation analysis

Major levels of boron in borosilicate glasses have been determined nondestructively by neutron activation analysis. In contrast to chemical methods for determining boron as a major component, the described nuclear method has few interferences and does not require chemical separation of boron prior to its quantitation. The effects of neutron self-shielding by boron (1 to 8% by weight) are examined, minimized by dilution of powdered samples with high purity graphite, and circumvented by comparative analyses. Results of the analysis of a series of glasses with increasing boron composition are 1.150±.005% and 7.766±.035% for the low and high members of the series. Accuracy of these results depends upon comparative analyses with the certified Standard Reference Material, SRM 93a (3.89±0.02% B). Once analyzed, the glasses are useful as secondary standards for alpha track counting, and also ion and electron microprobe analyses of glasses.     

The determination of minor elements in steel by proton-induced prompt gamma-ray spectrometry

Pure elemental targets of Si, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Mo and W were irradiated with protons from 3.5 to 6.0 MeV, interference-free sensitivities were calculated for analysis by prompt gamma-ray spectrometry and sensitivity curves were plotted to show the variation of sensitivity with bombarding energy. Appropriate bombarding energies were selected for analysis and the extent of possible inter-element interferences and background effects were determined. Standard reference steels were used to evaluate this method for the determination of the minor elements Si, V, Cr, Mn and Co.     

Elemental analysis of human placenta by neutron irradiation and gamma-ray spectrometry (standard,prompt and fast-neutron)

Human placental tissue from 100 hospitalized deliveries were analysed for Ag, Al, As, Au, B, Ba, Br, Ca, Cd, Cl, Co, Cr, Cs, Cu, F, Fe, I, Hg, K, La, Mg, Mn, Mo, Na, Ni, Rb, S, Sb, Sc, Se, Sn, Sr, Ti, V, W and Zn using a combination of pre-chemical separation of sodium with hydrated antimony pentoxide and instrumental neutron activation analysis. Boron and Si values were determined using prompt gamma-ray and fast-neutron techniques respectively. Analysis of NBS-SRM Bovine Liver 1577 and a pooled standard placental tissue for 33 elements showed a good agreement with most coefficients of variation less than or equal to 15%, and recoveries of 91–104%. Symmetrical distributions, were obtained for all elemental placental values. Only Cd(–) and Zn(+) showed statistically significant correlations with birth weight, gestational age and placental weight. The influence of cigarette smoking is considered a major factor in producing elevated cadmium levels in the placental tissue of smokers and passive smokers, and hence lower birth weights.     

Application of prompt gamma-ray spectrometry to helium-3-induced activation of boron

An assessment was made of the analytical potential of the exoergic reactions on boron, induced by³He⁺ beams. Possible interferences from C, N and O were studied. Gamma-rays originating from (³He, n), (³He, d), (³He, d), (³He, ) and Coulomb excitation were identified. Possible practical applications in boron studies are indicated.     

Determination of boron in marine carbonates by prompt gamma-ray analysis

Boron in carbonate reference samples was measured by neutron-induced prompt gamma-ray analysis (PGA) using cold and thermal neutron guide beams of the JRR-3M reactor. In order to determine B contents in marine carbonates, the Doppler-broadened -ray peak of 478 keV was used together with the correction of interference from Na-peak of 472 keV. We determined B in coral samples within 3% of analytical precision. The data obtained by the present method are mostly consistent with reported values. Here, we report PGA of B in marine carbonates.     

A brief review of the determination of cadmium by prompt gamma-ray neutron activation analysis

An examination of the literature concerning the determination of cadmium by Prompt Gamma-Ray Neutron Activation Analysis (PGNAA) has been conducted. In-vivo activation analysis of the liver and kidney is the most common application reported and is briefly reviewed here. This review will concentrate on the determination of cadmium in in-vitro systems. These include a number of different complex matrices such as geological, environmental and biological materials, as well as water, sediments, foods and construction material. Nuclear reactors, accelerators, and radioisotopes have all been used as neutron sources with varying degrees of sensitivity.     

Non-destructive determination of trace amounts of iodine in biological samples by epithermal neutron activation and Compton suppression gamma-ray spectrometry

In order to investigate the ingestion of iodine by human body and to know its content in organs, instrumental epithermal neutron activation analysis was used in conjunction with Compton suppression gamma-ray spectrometry by measuring the ¹²⁸I short-lived nuclide. The interferences of ²⁴Na and ³⁸Cl induced from NaCl in a sample were reduced by factors of about 6 and 15 to 41 by employing the epithermal neutron activation and Compton suppression gamma-ray spectrometry, respectively. The present method can be used to determine iodine at levels higher than 11 ppb. It was applied to the determination of iodine of more than 35 ppb in various biological reference materials.     

Determination of nitrogen in steels by alpha-induced prompt gamma-ray spectrometry

The prompt gamma-ray of 871 keV emitted during the bombardment of steels by 5 MeV alpha particles were used to determine nitrogen by means of the reaction¹⁴N(α, pγ)¹⁷O. The method is non-destructive, rapid and experimentally simple. It has a sensitivity of about 7 μg·g⁻¹. In the nitrogen concentration range of 10¹–10² μg·g⁻¹ the relative precision of the method is about 3%. The accuracy of the method compares with that of other nuclear methods. Presented at the 5th Symposium on Recent Developments in Activation Analysis, Oxford, 17–21 July, 1978.     

Analysis of boron in biological reference materials using prompt gamma activation analysis

Summary A prompt gamma activation analysis facility has been constructed on the ST1 horizontal beam port at the HANARO research reactor, KAERI in 2003. The detector system consists of a high-purity Ge detector surrounded by BGO/NaI(Tl) scintillators as an annulus type to reject the Compton scattered photons. Detection sensitivity for boron was obtained from the prompt gamma-ray spectra of boric acid, B(OH)₃, containing 0.1-65 μg boron. The net peak for the calculation of the boron concentration was obtained by eliminating the sodium 472 keV peak, involved in the boron 478 keV peak. The biological samples used are NIST SRMs such as Peach Leaves, Apple Leaves, Tomato Leaves, Spinach Leaves, Total Diet, Typical Diet, Oyster Tissue and Corn Bran, etc. The measured values for high boron concentration showed up to a 3% of the relative, but in a low concentration below 5 ppm, present values were higher than the certified ones.     

Intercomparison of inductively coupled plasma mass spectrometry, quantitative neutron capture radiography, and prompt gamma activation analysis for the determination of boron in biological samples

Boron determination in blood and tissue samples is a crucial task especially for treatment planning, preclinical research, and clinical application of boron neutron capture therapy (BNCT). Comparison of clinical findings remains difficult due to a variety of analytical methods, protocols, and standard reference materials in use. This paper addresses the comparability of inductively coupled plasma mass spectrometry, quantitative neutron capture radiography, and prompt gamma activation analysis for the determination of boron in biological samples. It was possible to demonstrate that three different methods relying on three different principles of sample preparation and boron detection can be validated against each other and yield consistent results for both blood and tissue samples. The samples were obtained during a clinical study for the application of BNCT for liver malignancies and therefore represent a realistic situation for boron analysis.     

Thallium determination in biological materials by radiochemical neutron activation analysis

Summary The determination of thallium in biological materials sometimes cause problems because of the low concentrations of this toxic element. In the present work a method is described which optimizes the parameters affecting the specificity and sensitivity of the radiochemical NAA of thallium in biological samples. High thermal neutron flux, complete decomposition of the organic matter by pressurized digestion, TlI precipitations, liquid extraction of HTlBr₄ and La(OH)₃ scavenging purification are the steps leading to the final homogeneous preparation of Tl₂CrO₄ for -activity measurement. The method was applied to various materials as bovine liver, bone and nails. Good agreement was found between certified and determined thallium concentrations of the reference material CRM 176. The chemical yield comes to about 80%, with low deviations. The sensitivity of the method is about 10^–3 g/g, the standard deviations being in the range of 3.6% (CRM 176), 14% (bovine liver), and 17% (bone). Detailed working instructions are given.     

Elemental concentrations in geochemical reference samples by neutron capture prompt gamma-ray spectroscopy

A facility for neutron capture prompt gamma-ray activation analysis, installed on a curved thermal neutron guide at the ILL High Flux Reactor, is described. Elemental sensitivities for B, Sm and Gd have been measured. The performance of the facility has been assessed by the measurement of these trace elements in eleven USGS geochemical reference samples and comparison of the results with existing values. Preliminary concentrations of B, Sm and Gd are also reported for twelve French GRS.     

Determination of boron in Japanese geochemical reference samples by neutron-induced prompt gamma-ray analysis

Determination of ppm levels of B in 21 igneous and sedimentary rocks of the Japanese geochemical reference samples prepared by the Geological Survey of Japan (GSJ) has been performed by neutron-induced prompt γ-ray analysis (PGA) using cold and thermal guided neutron beams of the JRR-3M. Owing to the Doppler broadened γ-ray line of B 478 keV, many elements such as Na, Ni, Cl and so on showed spectral interference in the determination of B. The interference was corrected by computer fitting and a reference peak method. The analytical results obtained by the present method almost agreed with the GSJ values recommended in 1994 within the standard deviation of the recommended values. Sodium contents determined by the PGA in the reference rock samples are also reported.     

The determination of10B by prompt proton spectrometry

Boron was analysed in ore and glass samples by prompt proton spectrometry, using deuterons of 2.7 MeV to coincide with a region where the excitation function of the¹⁰B(d, p)¹¹B reaction did not vary appreciably with energy. Targets of approximately 300 μg/cm² thick of powdered samples were prepared by centrifugation. Concentrations down to 0.2% were determined. Possible interference by other elements, particularly nitrogen, magnesium and titanium, was investigated.     

Simultaneous determination of boron,phosphorus and sulphur in some biological and soil materials by inductively-coupled plasma emission spectrometry

Atomic emission lines at 249.678 nm, 214.911 nm and 180.735 nm are used simultaneously to determine total concentrations of boron, phosphorus and sulphur respectively, in plant and soil sample digests by means of inductively-coupled plasma emission spectrometry. The digestion procedures chosen enable these elements to be determined simultaneously on a single digest. Analytical data are compared after using various digestion procedures on standard reference materials. Actual and potential interelement interferences in the plasma are discussed together with attempts to overcome these interferences. Limitations for simultaneous determinations of boron, phosphorus and sulphur remain in the digestion and dissolution procedures.     

Sensitive determination of traces of boron in waters,fertilizers na geological and biological materials by isotope-dilution mass spectrometry

A method is described for determining traces of boron in water, fertilizers, geological and biological (reference) materials by isotope-dilution mass spectrometry after separation on an Amberlite IRA-743 borate-selective ion-exchange column. Boron (–250 ng g^?1) in water can be determined with an accuracy of 5–20% (computed on a 2s basis). After correction for weighing errors and for moisture, content, which varied from 0 to 8% for the samples tested, 1–35 μg g^?1 boron in “dry” fertilizer, biological or geological sample can be assayed with an accuracy of 5–30% (2s). In an IAEA interlaboratory program on a simulated fresh water, the method yielded a value of 24.3 +? 2 μg l^?1, compared to the make-up value of 25 μg l^?1.