Total Reflection X-ray Fluorescence Technique Research Articles

Effect of sample carriers on analytical parameters in total reflection X-ray fluorescence - a tool for multi-trace elemental analysis

The Total reflection X-ray Fluorescence technique is increasingly popular for its simplicity and rapid elemental screening. This study evaluates the various analytical parameters including spectroscopic resolution, absolute sensitivity, relative element sensitivity, lowest limits of detection, accuracy and precision of the Total reflection X-ray Fluorescence spectrometer. This evaluation is conducted using quartz and acrylic sample carriers with mono and multi-element standards. Notably, the quartz sample carrier demonstrated excellent values of spectroscopic resolution, absolute sensitivity, the lowest limits of detection, a recovery rate of 90–110% and a coefficient of variation of 3–6% for the quantified elements from mono and multi-element standards. These findings underscore the robust analytical capability of the Total reflection X-ray Fluorescence technique for multi-trace elemental analysis. This research article not only provides practical and straightforward guidelines for handling Total reflection X-ray Fluorescence spectrometer but also confirms the practicality and effectiveness of the sample carriers for rapid and reliable elemental screening applications.

Total Reflection Xray Fluorescence (TXRF) spectrometry as a powerful and broad-spectrum analytical tool in the nuclear sciences

X-ray spectroscopy is widely used in nuclear reaction and structure studies. To aid such studies the technological envelope is continually being pushed to achieve higher quality such as superior power and brilliance, higher resolution and sensitivity. We present the discussion of a relatively new form of X-ray fluorescence spectrometry - Total Reflection X-ray Fluorescence (TXRF) spectrometry that can achieve analytical sensitivities of the order of parts per billion (ppb). An overview of the TXRF technique is presented and its utility for nuclear materials analysis discussed. Polarized Energy Dispersive X-ray Fluorescence (PEDXRF) spectrometry is also an XRF technique that can complement TXRFS where it may not be applicable. That scenario is discussed with respect to our results using PEDXRF on geothermal samples that serve to corroborate the recent findings of the Borexino Geoneutrino Experiment regarding the high Th, U concentrations in the earth’s mantle.

Total reflection X-ray spectroscopy based detection of uranium and thorium in phosphogypsum simulated by Monte Carlo method

Detection of trace amounts of uranium and thorium in phosphogypsum using total reflection X-ray fluorescence (TXRF) was addressed by Monte Carlo method (MCNP code, version 6.2). The simulated samples contained average concentrations of 238U (120 Bq/kg) and 232Th (40 Bq/kg), as well as 7 major components in oxide forms and other 11 heavy metals in trace amounts, commonly found in PG. It was found that, for a molybdenum target X-ray tube operating under total reflection condition and equipped with an SDD detector, the detection limit for uranium and thorium in the simulated multi-elemental sample are (1.42±0.04)ng and (1.03±0.02)ng, respectively. Based on parameters of certified solutions for uranium and thorium, and adding gallium as an internal standard element, calibration plots provided mass recovery from the multi-component sample with relative errors of 4.56% for uranium and 2.74% for thorium. Our results show that TXRF technique can accurately detect and quantify trace amounts of uranium and thorium in the presence of matrix effects without any pre-treatment of PG samples.

The New Markers of Early Obesity-Related Organ and Metabolic Abnormalities.

The objective of our study was to identify new markers related to excessive body adiposity and its early consequences. For this purpose we determined serum FGF-19 and FGF-21 concentrations in obese rats, whose role in the pathogenesis of obesity is not yet established. In addition, a total reflection X-ray fluorescence technique was applied to determine the elemental chemistry of certain tissues affected by obesity. Next, the new biochemical and molecular parameters were correlated with well-known obesity-related markers of metabolic abnormalities. Our obese rats were characterized by increased calorie consumption and body adiposity, hypercholesterolemia, elevated levels of liver enzymes and FGF-21, while the level of FGF-19 was reduced. Strong relationships between new hormones and established metabolic parameters were observed. Furthermore, we demonstrated that obesity had the greatest effect on elemental composition in the adipose tissue and liver and that rubidium (Rb) had the highest importance in distinguishing the studied groups of animals. Tissue Rb strongly correlated with both well-known and new markers of obesity. In conclusion, we confirmed serum FGF-19 and FGF-21 as useful new markers of obesity-related metabolic alternations and we robustly propose Rb as a novel indicator of excessive body adiposity and its early consequences. However, further investigations are encouraged to address this clinical issue.

Synthesis, Ligating Properties, Thermal Behavior, Computational and Biological Studies of Some Azo-transition Metal Complexes

Synthesis of new Fe(III), Co(II), Ni(II), and Cu(II) complexes of two azo ligands; 1-(phenyldiazenyl) naphthalene-2-ol (sudan orange R, HL1), and sodium 2-hydroxy-5-[(E)-(4-nitrophenyl) diazenyl]benzoate (alizarin yellow GG, HL2) have been reported. Stoichiometries of 1:2 and 1:3 (M:L) of the synthesized complexes were approved by total-reflection X-ray fluorescence technique (TXRF) and by elemental analyses. The geometry of complexes (octahedral and square planar) was typified by various spectroscopic, thermal, and magnetic techniques. The ESR spectroscopy showed that Cu(II) complexes are of different isotropic and rhombic symmetries with the existence of Cu–Cu ions interaction. TGA, DTA, and DSC analyses supported the multi-stage thermal decomposition mechanisms, where the thermal breakdown is ended by the formation of metal oxide in most cases. Moreover, chemical reactivity modeling using the density functional theory (DFT) method with the B3LYP/6–31 basis set, showed that metal complexes are more biologically active than their precursor ligands. The calculated lipophilicity character for metal complexes is in the range of 33.8–37.5 eV. Docking results revealed high scoring energy for [Fe(HL2)3].H2O complex and moderate inhibition strength of [Cu(L1)2].H2O complex versus 1bqb, 3t88, and 4esw proteins. Ultimately, the extent of biological effectiveness was endorsed experimentally against four microbial strains. The results are guidelines for toxicological investigations.Graphical

TL and OSL analysis of natural orange calcite crystal

The study presents TL and OSL characterization of orange calcite. It is known that calcite exhibits TL however its OSL emission is unwell studied. The morphological characterization was done by means of X-rays diffraction (XRD) technique and it was confirmed that the sample is a pure calcium carbonate. Total and traces elements were determined using Total Reflection X-Ray Fluorescence (TXRF) technique and several impurities were found as P (53070 mg/kg), S (877 mg/kg), K (442.1 mg/kg), Ca (118290 mg/kg), Fe (330.4 mg/kg), Cr (101.19 mg/kg), and Ni (115.01 mg/kg), also some trace impurities, as Cu (1.96 mg/kg) and Zn (1.30 mg/kg), Mn (57.21 mg/kg) were determined and they may have important role in the luminescent emission. Sample in powder form was irradiated with crescent doses of beta particles, in an interval of 5–25 Gy and showed TL peaks at approximately 93, 125, 162, 189 and 227 °C. An OSL response was verified and can be fitted using 3 components with decay constant values of 2.3, 10.0 and 77.4 s.

Total Reflection X-ray Fluorescence Analysis of Plasma Elements in Autistic Children from India.

Trace elements are essential for the human body's various physiological processes but if they are present in higher concentration, these elements turn to be toxic and cause adverse effect on physiological processes. Similarly, deficiency of these essential elements also affects physiological processes and leads to abnormal metabolic activities. There is a lot of interest in recent years to know the mystery behind the involvement of trace elements in the metabolic activities of autistic children suspecting that it may be a risk factor in the aetiology of autism. The present study aims to analyse the plasma trace elements in autistic children using the total reflection X-ray fluorescence (TXRF) technique. Plasma samples from 70 autistic children (mean age: 11.5 ± 3.1) were analysed with 70 age- and sex-matched healthy children as controls (mean age: 12 ± 2.5). TXRF analysis revealed the higher concentration of copper (1227.8 ± 17.8), chromium (7.1 ± 2.5), bromine (2695.1 ± 24) and arsenic (126.3 ± 10) and lower concentration of potassium (440.1 ± 25), iron (1039.6 ± 28), zinc (635.7 ± 21), selenium (52.3 ± 8.5), rubidium (1528.9 ± 28) and molybdenum (162,800.8 ± 14) elements in the plasma of autistic children in comparison to healthy controls. Findings of the first study from India suggest these altered concentrations in elements in autistic children over normal healthy children affect the physiological processes and metabolism. Further studies are needed to clarify the association between the altered element concentration and physiology of autism in the North Karnataka population in India.

Орчны дээжинд микроэлемент хортой хүнд метал, цацраг идэвхт изотоп тодорхойлох

The present report outlines the activities in Environmental studies at Nuclear Research Center, National University of Mongolia, Ulaanbaatar. The Nuclear and Related Analytical Techniques, which developed in this center, played on very important role in Environmental studies due to several advantageous features as multielemental, accuracy and low detection limits of these methods. The most appreciated advantageof Gamma Spectrometric, with HP Ge detector and Total Reflection X-Ray Fluorescence Techniques are briefly reviewed and • the results on determination toxic heavy metals, trace, natural and man-made radioactive elements in aerosols, soil, water, food and hair samples are discussed in detail. Also, in this report give some results of natural radioactive measurements of soil, building materials and indoor's radon data in Erdenet and Ulaanbaatar cities. In some soil samples of Western Mongolia observed man-made radioisotope Cs-137 14.7-64.8 Bk/kg. It means the Western Mongolia exposed ground and air nuclear explosions at Semipalatinsk (Russia) and Lobnor (China).

Investigation of Soils and Pine Needles Using WDXRF and TXRF Techniques for Assessment of the Environmental Pollution of Shelekhov District, Eastern Siberia, by the Aluminum Industry and Heat Power Engineering

X-ray fluorescence analysis was applied to assess the ecological state of the area potentially polluted by emissions of the aluminum industry and heat power engineering. Soil and pine needle samples were collected in areas with industrial activity and analyzed using wavelength-dispersive X-ray fluorescence (WDXRF) and total-reflection X-ray fluorescence (TXRF) techniques. Both techniques were validated using the matrix-matched certified reference materials. Different sample preparation procedures, such as fusion and pressing for WDXRF and acid digestion and suspensions for TXRF as well as quantification approaches (the external calibration for WDXRF and the internal standard for TXRF) were applied according to the features of the analyzed samples. The rock-forming oxides (Na2O, MgO, Al2O3, SiO2, P2O5, K2O, CaO, TiO2, MnO, and Fe2O3) and trace elements (V, Cr, Ni, Cu, Zn, Rb, Sr, Y, Ba, and Pb) were quantified in soils, as well as several elements (Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, Pb, and Ba) were quantified in pine needles. Comparing the results of soils and pine needles analysis with the regional background values indicated a significant contamination pollution level of the studied area.

Effect of elemental composition assigned to antrotopic pollution on the quality of the water and sediment of the Marrecas river (PR, Brazil) as highlighted by multivariate statistical analyses

In recent years, several environmental pollutants have been monitored in surface waters and sediments. However, few studies apply multivariate statistics to identify the main components and correlate them temporally and spatially. In this sense, the present study sought to monitor the quality of water and sediments in the Rio Marrecas/Brazil, through the analysis of physicochemical parameters and trace elements, as well as to identifying sources of contamination, using multivariate statistics. For this purpose, sampling was carried out in nine locations for a period of 12 months. The Total Reflection X-ray Fluorescence (TXRF) technique was used to quantify the 15 elements identified in water and sediment samples. Through multivariate statistical analyses, the most significant elements, their correlations and possible pollutant sources were defined, and the pollution index (HPI) and assessment index (HEI) of heavy metals were applied. The parameters pH and BOD5 do not comply with Brazilian legislation. Based on PCA and Spearman correlation, there was strong evidence of contamination of the water naturally, composed of the elements Ti, V, Mn, Fe, and of anthropogenic origin composed of the elements Ca, Ni, Cu, Zn. These findings provide insights to determine the impacts of heavy metals on human health and the environment.

Determination of Elements due to Atmospheric Deposition on Barbula indica Moss at Dalat, Vietnam using NAA and TXRF Techniques

In this paper, two multielement analysis techniques, Neutron Activation Analysis (NAA) and Total Reflection X-ray Fluorescence (TXRF), are combined to detect elemental concentrations in Barbula indica moss collected at Dalat, Vietnam. Combining these two techniques has improved the qualitative detection of elements due to atmospheric deposition on moss samples. The concentrations of 40 elements, including Na, Mg, Al, Si, P, S, Cl, K, Ar, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Kr, Rb, Y, Sb, I, Cs, Ba, La, Ce, Sm, Eu, Tb, Dy, Yb, Hf, Ta, Pb, Th, and U in the Barbula indicamoss samples collected at 19 locations at Dalat have been determined. It is shown that the air in Dalat is suspected of contamination by Na, Mg, Si, P, S, V, Mn, Cu, Se, Br, and U; slightly contaminated by Mg, Cl, K, Cr, Ni, S, and Ni; moderately contaminated by Sc, Fe, Co, Zn, As, Kr, Rb, Y, Sb, Cs, Ba, La, Ce, Sm, Eu, Dy, Yb, Ta, Pb, and Th; and seriously contaminated by Tb. Factor analysis has been used to explain the contamination sources of these elements, including V, As, Fe, Zn, Se, Rb, Sb, Cs, Al, Cu, and Pb in the investigated area. Four factors have been extracted that can explain 86% of the total variance, and the results suggest that the main sources of atmospheric pollution in Dalat originate from traffic and windblown dust.

Determination of some elements in the nails in patients with colon cancer using total reflection X-ray fluorescence

Sixty-two subjects (31 men with colon cancer) participated in this study. The analysis of elements in the nails was performed by total reflection X-ray fluorescence (TXRF) technique. The results showed that fifteen elements were quantified, including the following: S, P, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, and Br. We have found that there were significant differences in the concentrations of elements Ca, Cr, Fe, Cu, Zn, As, and Se between normal subjects and men with colon cancer (p < 0.05). We conclude that TXRF is a technique suitable for elemental analysis in human nail samples. The concentration of elements Ca, Cr, Fe, Cu, Zn, As, and Se could be among the factors used for the diagnosis of colon cancer risk in men.

Methodology development and optimization for direct quantification of total selenium concentration in mine water by total-reflection X-ray fluorescence spectrometry

Methodology for direct quantification of total selenium (Se) concentration in mine water by total-reflection X-ray fluorescence (TXRF) spectrometry was developed and optimized. Inductively coupled plasma – mass spectrometry (ICP-MS), as a recognized standard test method, was used as a benchmark for results verification. Preliminary measurements with aqueous multi-element standard solutions showed that Se concentration can be accurately determined down to 10 ng/g by using a single-drop of solution (10 μL) and a measurement time of 600 s. Quantification of lower Se concentration below 10 ng/g was subsequently optimized, also with aqueous multi-element standard solutions. Improvement in detection limit was accomplished by increasing amount of sample deposition as well as increasing measurement time. TXRF analysis of SRM1640a, Trace Elements in Natural Water, was also performed for accuracy check. The developed methodology was applied to analyze five raw mine water samples (MW-1, MW-2, MW-3, MW-4 and MW-5) collected from anonymous mine site locations. TXRF analysis was performed on the as-received samples directly without filtration, dilution and digestion. Samples were prepared as single-drop specimens and analyzed using a measurement time of 600 s. Se and fifteen other elements were detected in varying degree in the as-received samples. Se concentrations quantified by TXRF were 256.5 ± 22.5, 88.4 ± 1.4 and 61.3 ± 2.8 ng/g for mine water samples MW-1, MW-2 and MW-3, respectively, compared to 255.3 ± 5.6, 87.3 ± 2.6 and 59.7 ± 3.5 ng/g by ICP-MS. No clear Se-Kα peak above background was observed for samples MW-4 and MW-5. Increasing amount of sample deposition by preparing triple-drop specimens and using a longer measurement time of 1800 s, allowed a Se-Kα peak to emerge above the background for MW-4, but not MW-5. Se concentration in MW-4 quantified by TXRF was 4.9 ± 0.5 ng/g, compared to 6.7 ± 0.7 ng/g by ICP-MS, which represents an agreement within three standard deviation values between the two techniques. For sample MW-5, even after using triple-drop specimens and increasing the measurement time to 1800 s, Se concentration could not be determined because a Se-Kα peak was not detected by TXRF, compared to the Se concentration of 0.83 ± 0.1 ng/g obtained by ICP-MS. Overall, our analysis results showed that the TXRF technique can be used for direct analysis of total Se concentration in raw mine water samples down to ng/g range, providing high-quality, accurate and repeatable analysis comparable to ICP-MS while requiring much simpler sample preparation.

Characterization of archaeological ceramics from eastern Siberia by total-reflection X-ray fluorescence spectrometry and principal component analysis

The study of the composition of archaeological ceramics provides information used to assess possible transportation routes and cultural connections between ancient people living in different regions. Total-reflection X-ray fluorescence (TXRF) was applied for the analysis of ceramics as a promising method due to the rapidity, cost-efficiency, and capability to analyze a very small amount of a sample (<20 mg), which is important for the preservation of archaeological material. Two techniques of sample preparation for the TXRF analysis of ceramics have been considered. The analysis of suspensions was applied to obtain information on the bulk composition of ceramics. Acid leaching was used for the elemental analysis of the clay component of the ceramics, with the separation of non-soluble mineral phase. The proposed TXRF techniques have been successfully validated by the analysis of reference material and comparison with independent analytical methods. Reproducibility (interlaboratory precision) was evaluated for the proposed TXRF leaching method involving two different laboratories. The application of grazing incidence X-ray fluorescence (GI-XRF) showed homogeneous distribution of elements in the specimen and correspondence of the measurements to the conditions of total external reflection. TXRF method was applied to collect the first data on the composition of archaeological samples of ceramics from Popovsky Lug, eastern Siberia (Russia). The obtained data on the elemental composition were used to classify the samples by statistical methods of analysis, including the method of principal components and factor analysis. Three different compositional groups of ceramic have been separated and accepted as corresponding to archaeological interpretation.

X-ray Fluorescence Techniques in Determining the Habitat Preferences of Species-Ulva pilifera (Ulvales, Chlorophyta) from Montenegro Case Study.

The paper presents four new sites where bright green Ulva thalli were found inhabiting freshwater (a river, a ditch, the Milet Canal) and marine (on the rocky shore of the Adriatic Sea) habitats in Montenegro. The aims of this study were to determine, for the first time, whether specimens of Ulva pilifera collected in Montenegro are phylogenetically and morphologically the same species as the one occurring in Europe. Using total reflection X-ray fluorescence (TXRF) and wavelength dispersive X-ray fluorescence (WDXRF) techniques it assessed the elemental composition of their thalli and its influence to colonise new habitats. Elements: Al, As, Ba, Br, Ca, Cl, Cr, Cu, Fe, Hf, I, K, Mg, Mn, Na, Ni, P, Pb, Rb, S, Si, Sr, Ti, V, and Zn were determined. The highest elemental concentrations were found for Ca = 16.3% (using WDXRF) and for Sr = 292 ppm (using TXRF) in the Ulva thalli. Ulva pilifera analysed from Montenegro, based on classical morphological methods and molecular techniques, are closely related to the same species from inland and coastal waters throughout Europe. The analysis of trace elements showed that the metal content in Ulva thalli is correlated with the trace elements in water and sediments. Ulva pilifera fits numerous features that make it one of the bioindicators of marine pollution, thanks to its worldwide distribution and capacity to accumulate trace elements.

Relationship of levels of trace elements in saliva and dental caries in preschool children using total reflection X-ray fluorescence technique (TXRF)⋆

BackgroundConsidering that studies on the relationship between dental caries and trace elements present contradictory and inconclusive results, the purpose of this study was to determine the levels of salivary trace elements in saliva samples of preschool children and investigate their relationship with dental caries. MethodsIn total, 120 samples of unstimulated saliva were collected from children aged 36–72 months, of both sexes, who participate in the preventative educational program in oral health at the State University of Londrina, Brazil. The children were divided into two groups, caries (n = 60) and non-caries (n = 60). Levels of Al, Cu, Fe, Mn, and Zn were analyzed by total reflection X-ray fluorescence (TXRF). Descriptive statistics, the Student’s t-test, Mann-Whitney U test, and Pearson’s Chi-squared test were performed (P < 0.05). ResultsThe concentrations of Mn and Fe were significantly higher in the caries group (Mn =0.015 mg/L [0.007−0.020]; Fe =0.080 mg/L [0.031−0.239] than the non-caries group (Mn =0.010 mg/L [0.001 – 0.017]; Fe =0.044 mg/L [0.023 – 0.107]). ConclusionThe results suggest a relationship between trace elements and dental caries, indicating possible involvement of these elements in the metabolism of microorganisms involved in the carious process. In addition, the use of TXRF presented satisfactory results, with a simple and fast methodology for the detection of the studied elements.

Application of TXRF in monitoring trace metals in particulate matter and cloud water

Abstract. Trace metals in ambient particulate matter and cloud are considered key elements of atmospheric processes as they affect air quality, environmental ecosystems, and cloud formation. However, they are often available at trace concentrations in these media such that their analysis requires high-precision and sensitive techniques. In this study, different analytical methods were applied to quantify trace metals in particulate matter (PM) samples collected on quartz and polycarbonate filters as well as cloud water, using the Total reflection X-Ray Fluorescence (TXRF) technique. These methods considered the measurement of filter samples directly without and with chemical pretreatment. Direct measurements involved the analysis of PM samples collected on polycarbonate filters and cloud water samples after they are brought onto TXRF carrier substrates. The chemical treatment method involved the assessment of different acid digestion procedures on PM sampled on quartz filters. The solutions applied were reverse aqua regia, nitric acid, and a combination of nitric acid and hydrogen peroxide. The effect of cold-plasma treatment of samples on polycarbonate filters before TXRF measurements was also investigated. Digestion with the reverse aqua regia solution provided lower blanks and higher recovery in comparison to other tested procedures. The detection limits of the elements ranged from 0.3 to 44 ng cm−2. Ca, K, Zn, and Fe showed the highest detection limits of 44, 35, 6, and 1 ng cm−2, while As and Se had the lowest of 0.3 and 0.8 ng cm−2, respectively. The method showed higher recovery for most trace metals when applied to commercially available reference materials and field samples. TXRF measurements showed good agreement with results obtained from ion chromatography measurements for elements such as Ca and K. Cold-plasma treatment did not significantly lead to an increase in the detected concentration, and the results were element specific. Baking of the quartz filters prior to sampling showed a reduction of more than 20 % of the filter blanks for elements such as V, Sr, Mn, Zn, and Sb. The methods were applied successfully on ambient particulate matter and cloud water samples collected from the Atlas Mohammed V station in Morocco and the Cape Verde Atmospheric Observatory. The obtained concentrations were within the range reported using different techniques from similar remote and background regions elsewhere, especially for elements of anthropogenic origins such as V, Pb, and Zn with concentrations of up to 10, 19, and 28 ng m−3, respectively. Enrichment factor analysis indicated that crustal matter dominated the abundance of most of the elements, while anthropogenic activities also contributed to the abundance of elements such as Sb, Se, and Pb. The results confirm that TXRF is a useful complementary sensitive technique for trace metal analysis of particulate matter in the microgram range as well as in cloud water droplets.

An assessment of landfill leachate influences on water quality in the Boi Piguá river basin (Paraná, Brazil) using the TXRF technique

In this study, strong evidence of anthropic pollution was identified in the waters of the Boi Pigua River near the municipal landfill of Cascavel-PR. The elemental composition of the river water from five collection sites, the groundwater from four sites and the municipal landfill leachate were monitored over 1 year, using the total reflection X-ray fluorescence (TXRF) technique. Ten elements (Cl, K, Ca, Ti, Mn, Fe, Ni, Cu, Zn, and Ba) were identified in the water samples. The elemental concentration data set was reduced to specific variabilities and characteristic clusters by applying cluster and principal component analysis (PCA). The greatest variability in concentration was observed in the Mn and Ba data, which formed the first, main component. A further three principal components were needed to explain the variability in the Ni, Cu, and Fe concentrations. According to the cluster analysis, samples from all the river and water table collection sites shared similarities with the landfill leachate composition. Thus, it is possible to affirm that the quality of the Boi Pigua River water has undergone major changes and an immediate intervention of environmental agencies is required.

Development of Methods to Evaluate Several Levels of Uranium Concentrations in Drainage Water Using Total Reflection X-Ray Fluorescence Technique.

As a country's law stipulates the effluent standard uranium concentration in drainage water, the uranium concentration must be determined when drainage water is released from a uranium handling facility, such as the Fukushima Daiichi nuclear power plant. The maximum allowable limit for uranium release at each facility is defined taking into consideration the situation of the facility, such as 1/10 to 1/100 of this effluent standard value. Currently, the uranium concentration of drainage water is commonly determined by α-particle spectrometry, in which several liters of drainage water must be evaporated, requiring about half of a day followed by 2–3 h of measurements, due to the low specific radioactivity of uranium. This work proposes a new methodology for the rapid and simple measurement of several levels of uranium in drainage water by a total reflection X-ray fluorescence (TXRF) analysis. Using a portable device for TXRF measurements was found to enable measurements with 1/10 the sensitivity of the effluent standard value by 10 times condensation of the uranium-containing sample solution; a benchtop device is useful to measure uranium concentrations <1/100 of the effluent standard value. Therefore, the selective usage of methods by a portable and benchtop devices allows for screening and precise evaluation of uranium concentrations in drainage water.

Chemical Analysis of Air Particulate Matter Trapped by a Porous Material, Synthesized from Silica Fume and Sodium Alginate

This work shows the ability of a new porous material (SUNSPACE), obtained by industrial by-products, to sequestrate air particulate matter (PM). This activity allows introducing the azure chemistry approach, devoted to better link new remediation strategies and sustainability. In particular, SUNSPACE is synthesized from silica fume and sodium alginate; it can be shaped in a porous solid, and it looks promising for environmental application as nanoparticle sequestration. Studies to evaluate the sequestration capability of SUNSPACE are performed in different environments, with and without anthropogenic sources of PM. Solid SUNSPACE disc samples are used as passive samplers and exposed for one and two months, in vertical and horizontal positions, indoor, and outdoor. Total reflection X-ray fluorescence technique is employed to perform elemental chemical analysis of the entrapped PM. Two sample preparation strategies to evaluate the composition of PM are considered: sample sonication in Milli-Q water and total sample mineralization by microwave acid digestion. These two options are proposed to analyse different PM fractions: in particular, sonication allows removing the coarse PM, entrapped on external material surface pores; on the contrary, digestion can offer information on fine and ultrafine PM, trapped in internal pores. Results confirm the ability of the porous material to sequestrate air PM and the differences in the sample preparation, supported by elemental analysis, and show the difference in the coarse and fine air particulate matter composition. In summary, the new material results as very promising for applications requiring nanoparticle sequestration.