Inductively coupled plasma mass spectrometry (ICP-MS) and instrumental neutron activation analysis (INAA) were applied to study the elemental content of coal combustion residues. Both methods’ analytical applicability and suitability for this type of material were described in detail. A certified reference material, fine fly ash (CTA-FFA-1), was used to examine the capabilities and validation of both methods. A comparison study allowed for the modification of the procedures for these materials (previously elaborated in the Institute of Nuclear Chemistry and Technology), resulting in more accurate data with lower uncertainty. We highlighted that INAA and ICPs complemented each other in the analysis of coal and coal combustion residues. The digestion procedure was an integral part of the measurement and affected the environmental analysis results. Both methods were applied to the chemical characteristics of coal ashes from household furnaces. The hard coal was from Polish, Columbian, and Kazakh mines. The majority of elements had similar concentrations, independently of coal origin. Because ash from domestic coal combustion is used as a fertilizer or an anti-icing agent, we assessed the potential environmental impact via leaching experiments (according to PN-EN 12457-2). The potential risk of soil contamination due to ash dumping around the house and its surroundings was determined as insignificant (for the elements investigated).

High temperature gas-cooled reactors have recently gained importance as a source of electricity and process heat. Nuclear fuel used in these reactors consists of TRISO (TRiple coated ISOtropic) coated particles, where spherical grains of UO₂ or UC₂ or UCO kernel are covered with four successive layers consisting of pyrolytic carbon and silicon carbide. Of great importance is the chemical purity of reagents and substances used for the production of TRISO coated fuel particles. Analytical techniques ensuring the determination of elements at trace levels are inductively coupled plasma mass spectrometry (ICP-MS) and neutron activation analysis (NAA). They were applied in this work for the chemical characterization of substrates used for TRISO fuel production. Two analytical procedures were developed: the first, where materials are analyzed using ICP-MS, and the second with the aid of NAA. Successive stages of these procedures are described with details. Results of quantitative chemical analysis of examined substances are reported as well as detection limits for the investigated elements. Moreover, the expanded uncertainties estimated for the determined elements while employing the devised analytical procedures are presented.

Solvent extraction of metals from Ti ore was investigated with a view of enhancing extraction yields by changing the concentration of the ligands, the rate of mixing, the pH, and the temperature of the solution. Norwegian Ti ore was leached with 5M HNO₃ alongside 10% ascorbic acid to obtain a pregnant solution containing transition metals and some rare earth elements (REEs). Part Two of the study will address the recovery of the REEs in the ore. The elemental analysis of solid and aqueous samples was done by two models of total reflection X-ray fluorescence spectrometers (S2 PICOFOX, Bruker Corporation, Berlin, Germany; and T-STAR, Bruker Corporation, Berlin, Germany). The same analysis was repeated using an inductively coupled plasma-mass spectrometer (Perkin Elmer Sciex ELAN DRC II, Perkin Elmer, Waltham, MA, USA). The extraction process and parameters were examined by ICP-MS. The extraction efficiencies were studied under different conditions through the use of various concentrations of ligands at different pHs, temperatures, and mixing rates of the solution. At pH 1.0, 22.5 °C, and a mixing rate of 1400 rpm, the selectivity of 150 g/L trioctyl methyl ammonium chloride (Aliquat 336) was 99% Ti⁴⁺, 94% V⁴⁺, and 82% Hf⁴⁺, while 99% of Co²⁺ was recovered at pH 0.8. The extraction efficiency of triethyl phosphate (10% TEP) was 58% Cu²⁺, 68% Mn²⁺, and 63% V⁴⁺ at 55 °C, 1400 rpm, and without a pH change. Tributyl phosphate (10% TBP) was able to retrieve 87% Cu²⁺ and 78% Zn²⁺ at pH 1.3, 1400 rpm, and 22.5 °C, and 80% Ti⁴⁺ at pH 1.2. A 10% solution of 2,4,6-tris (allyloxy)-1,3,5-triazine (TAOT) demonstrated 61% Mn²⁺ and 56% Hf⁴⁺ extraction at pH 1.3, 22.5 °C, and 1400 rpm. Under the same conditions, 10% methyl salicylate (MS) was able to recover 56% Hf⁴⁺ at pH 1.3. Using 1400 rpm, di (2-ethylhexyl) phosphoric acid (10% D2EHPA) was found to selectively extract 87% Hf⁴⁺ at 22.5 °C without a pH change, and around 99% Co²⁺, Ti⁴⁺, and Fe²⁺ at pH 1.3. This study provides valuable insights into optimizing solvent extraction conditions for transition metals’ recovery and serves as a precursor to future research on the extraction of REEs from Ti ores. This process is relevant from the environmental and economic perspectives since it provides the best approach to recycling metals to reduce the rate of raw ore mining.

This work reports the possibility of uranium recovery from a post-mining uranium ore dump in Poland by a bioleaching method. The studies were conducted on the dump leaching model with the mass of 570 kg of uranium bearing mineral material from Radoniów pile and in the periodic bioreactor with a work volume of 80 dm³ and with mechanical mixing and aeration of the charge. The uranium concentration in the examined material was about 800 ppm. In this process, the consortium of microorganisms isolated from former mines was used. It was composed of the following microorganisms: Bacillius, Pseudomonas, Sphingomonas, Thiobacillus, Halothiobacillus, Thiomonas, and Geothrix. The efficiency of the uranium bioleaching process was 98% in the reactor, and a yield of 70% was obtained in the dump leaching model. The post-leaching solution contained significant amounts of uranium ions that were separated in two stages: (1) by ion chromatography and then (2) by a two-step precipitation method. The resulting solution was a source of ammonium diuranate, the precursor of yellowcake (uranium oxides).

With advancements in hardware and software, non-destructive radiometric analytical methods have become popular in a wide range of applications. A typical case is the study of the leaching process of metals from mineral ores and mine tailings. The objective of the current study was to develop a radiometric method based on neutron activation analysis (NAA), in particular, delayed gamma neutron activation analysis (DGNAA), to monitor the process of Mn and Zn leaching from Ti ore, Cu mine tailings, and Zn-Pb mine tailings. The DGNAA method was performed using a neutron source: a deuterium-tritium (D-T) neutron generator for Mn and a MARIA research nuclear reactor for Zn. Laboratory-scale Mn leaching from Ti ores, Cu tailings, and Zn-Pb tailings was investigated using delayed gamma-rays of ⁵⁶Mn (half-life of 2.6 h). The dissolution efficiencies of Mn were found to increase with interaction time and HCl concentration (1 to 5 M) and to vary with the leaching temperature (22.5 to 110 °C). Such results were found to agree with those obtained by total reflection X-ray fluorescence (TXRF) spectrometry for the same samples. ⁶⁵Zn (half-life of 244 days) was chosen to investigate real-time/online leaching of Zn in Ti ore, Cu tailings, and Zn-Pb tailings. During online monitoring, Zn recovery was also reported to increase with increased leaching time. After approximately 300 min of leaching, 80%, 79%, and 53% recovery of Zn in Zn-Pb tailings, Ti ore, and Cu tailings, respectively, were reported. Theoretically, developed mathematical prediction models for ⁶⁵Zn radiotracer analysis showed that the spherical diffusion model requires much less time to attain saturation compared to the linear diffusion model. The results of NAA for Zn were compared with those obtained by handheld X-ray fluorescence (handheld-XRF) and TXRF analysis. The analyzed samples encompassed leached Ti ore, Cu tailings, and Zn-Pb tailings which were subjected to different conditions of leaching time, temperature, and HCl concentrations. The XRF analysis confirmed that the leaching efficiencies of Zn rise with the increase in leaching time and HCl concentration and fluctuate with leaching temperature. The developed approach is important and can be applied in laboratories and industrial setups for online monitoring of the recovery of any element whose isotopes can be activated using neutrons. The efficiency of the metal-recovery process has a direct impact on the normal operation and economic advantages of hydrometallurgy.