In the paper results of single- and double-pulse LIBS (Laser-Induced Breakdown Spectroscopy) measurements in collinear geometry are described. The experiments were performed using a unique self-made Nd:YAG laser operating in the Q-switching regime, where the laser transmission losses are switched. Such a laser allowed for an easy and quick change of the operating mode (one and two pulses), free shaping of the energy ratio of the two pulses (division of the energy of a single pulse into two parts) and a smooth change of the delay time between pulses in the range from 200 ns to 10 μs. To our knowledge, such a laser was used in LIBS measurements for the first time. LIBS experiments revealed strong self-absorption depending on energy ratios carried out in the first and second laser pulse in the double-pulse mode. This was confirmed also by statistical factorial analysis of LIBS spectra. Plasma temperature and LIBS signal enhancement were measured both for energy proportions between the first and the second laser pulse and for the first-to-second-pulse delay.
Lead 210Pb, an element of the natural uranium radioactive decay series, is not currently considered a source of radiation risk, especially in a radiation protection system in underground mines in Poland. However, it could be a completely independent element of the radioactive series due to its physical and chemical properties. Routine measurements showed significantly higher than expected concentrations of 210Pb in underground radium rich sediments, based only on the radioactive decay law. This phenomenon implies a need of 210Pb concentration monitoring in such sediments. Nevertheless, the laboratory analysis of 210Pb by gamma radiation spectroscopy is connected with a particular hindrance, the self-attenuation of 210Pb radiation in samples. Current work describes a practical method for obtaining the self-attenuation correction factor in the case of 210Pb concentration analysis. Experimentally obtained correction factors range between 0.51–6.96 cm2/g. Neglecting this factor can cause a significant error or underestimations in radiological risk assessment.
PL
Izotop 210Pb, element naturalnego szeregu promieniotwórczego 238U, jak dotąd nie był uwzględniany przy ocenie ryzyka zagrożenia radiacyjnego, szczególnie w odniesieniu do systemu ochrony radiologicznej w podziemnych zakładach górniczych (Rozporządzenie 2002) czy kontroli narażenia radiacyjnego związanego z wydobyciem oraz przetwórstwem ropy i gazu (Radiation... 1999). Okazuje się jednak, że ze względu na swoje właściwości fizykochemiczne nuklid ten może zachowywać się zupełnie niezależnie od pozostałych elementów szeregu, w którym występuje. Wyniki badań prowadzonych w ramach rutynowej kontroli zagrożenia radiacyjnego w podziemnych zakładach górniczych świadczą o tym, że dla większości osadów dołowych, powstających na skutek współstrącenia radu i baru w postaci siarczanu radowo-barowego, obserwuje się znacznie wyższe jego stężenia, niż wynikałoby to z samego tylko rozpadu 226Ra. Implikuje to konieczność monitorowania stężenia 210Pb w tych osadach, co jest związane z wieloma trudnościami analitycznymi i pomiarowymi. Niniejszy artykuł poświęcony jest wyznaczaniu współczynnika poprawkowego związanego ze zjawiskiem samoabsorpcji w próbkach stałych podczas oznaczania 210Pb metodą spektrometrii promieniowania gamma. Uzyskane współczynniki wahały się w granicach 0,51–6,96 cm2/g, co dowodzi, że nieuwzględnienie poprawki na samoabsorpcję, może prowadzić do poważnych błędów i niedoszacowań w ocenie zagrożenia radiacyjnego.
In this work empirical functions which relate the full-energy peak efficiency with sample height, energy, matrix composition and bulk density for voluminal samples in a cylindrical counting geometry were found. Accurate determination of the radioactivity of gamma-emitting radionuclides in environmental samples requires taking into account self-absorption. For the obtained self-absorption correction factor, a direct transmission method was chosen. Finally, this paper proposes a simple correlation between the self-absorption correction factor and the bulk density and height of the measured sample for a given energy.
The paper outlines the methodology used in the Gamma-Ray Spectrometry Laboratory for high-precision measurements of radionuclide activity concentrations in environmental samples. The Laboratory equipment includes a semiconductor detector HPGe with a 42% relative efficiency. The detector is placed in a Pb housing made of bricks 10 cm in thickness. Three measurement geometries are considered: Marinelli beakers 710 cm3 in volume and two cylindrical geometries 121 and 48 cm3 in volume. In the efficiency calibration (E = 32 division sign 1836 keV) mixed gamma standard solutions were used. Obtained experimental efficiency values epsilon were fitted with two quadratic functions. The junction point is that equivalent to 200 keV. Uncertainty of the calibration curve is 2% for E > 200 keV. The relationship between the total efficiency and the energy epsilon t(E) was also found for energies E = 33 division sign 1250 keV. Self-absorption correction factors Cs are calculated by the method proposed by K. Debertin, the uncertainty level being 1 division sign 2% for E > 100 keV. These correction factors are calculated by an original computer program. Coincidence summing correction factors Cc for the selected nuclides are derived using the ETNA computer program, basing on the relationships epsilon(E) and epsilon t(E). Minimum detectable activity (MDA) for selected nuclides encountered in environmental samples was determined for the water matrix. The methodology used was successfully verified in the course of international intercomparison measurements.
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To assure quality measurements, the algorithms used in data analysis need to be demonstra-bly correct. In practice, however, some less transparent or more complicated algorithms may be difficult to trace back to their original derivation. We point out that a commonly cited publication in neutron self-shielding is in need of correction in some details.
PL
Zapewnienie jakości pomiarowej wymaga aby algorytmy stosowane do analizy danych były w oczywisty sposób wolne od błędów. Jednakże w praktyce bywa, że trudno jest dotrzeć do pierwotnego wyprowadzenie niektórych mniej przejrzystych lub bardziej skomplikowanych algorytmów. W niniejszej pracy wskazujemy, że pewna powszechnie cytowana publikacja na temat efektu samoosłaniania neutronów wymaga poprawienia w niektórych szczegółach.
Of major concern are the self-absorption correction factors Cs in precise gamma-ray spectrometry of environmental samples. The overview of Cs determination methods (experimental, Monte Carlo calculations, analytical function application) is presented. Among several available methods, the author chose the one proposed by Debertin where the uncertainty level of Cs correction factor is 1÷2%. The point-like detector model is assumed whilst its efficiency is taken to be proportional to the weighted sum (integral) of the number of photons coming from sample volume elements. Computer program was developed to support the computation of Cs by the Debertin's method for samples in cylindrical geometries and Marinelli beakers. The input data are sample dimensions, density and the mass attenuation coefficient. The Cs uncertainty due to an arbitrarily chosen position of a point-like detector would not exceed 1% for the considered photon energies and the sample density range. Utilising this computer program, the relationships Cs(E,ń) were obtained for the applied geometries and a SiO2 matrix to support routine measurements. The SiO2 matrix is widely encountered in environmental spectrometry. This relationship was derived by fitting the computed data with the function Cs(E,ń) in the form proposed by Bolivar. It was shown that while handling this function to samples with the H2O matrix, the error involved in estimations would not exceed 3%.
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