Portable XRF Spectrometer Research Articles

Determination of Fe in blood using portable X-ray fluorescence spectrometry: an alternative for sports medicine

An alternate methodology based on a portable X-ray fluorescence spectrometry (PXRFS) for determination of Fe in blood was evaluated. The iron concentrations was determined in whole blood of 18 male amateur athletes (runners) using this portable XRF spectrometer and compared with a control group (54 male donors at the same age but not involved with physical activities) obtained by XRF and NAA techniques. The Fe concentration in the blood of runners is an important factor in sports medicine contributing to the performance of endurance athletes as well as for proposing new protocols of clinical evaluation.

The native development of ancient Chinese glassmaking: a case study on some early lead-barium-silicate glasses using a portable XRF spectrometer

In this paper, a portable energy-dispersive X-ray fluorescence spectrometer was used for the nondestructive analysis of 41 lead–barium–silicate glass artifacts dated from the Warring States Period to the Han Dynasties (475 BC–220 AD). These glasses mainly are ornament, funeral and ritual vessels unearthed from different provinces of China. Based on the chemical compositions obtained, the affects of surface weathering on the quantitative results, the characteristics of chemical compositions and the colorants were discussed. Meanwhile, referred to the research results reported and historical background, the raw materials, the distribution, the cause, the origin and the production center of the lead barium glass were also discussed. The present research provides new valuable information for tracing the origin and transfer of glassmaking techniques of ancient China. Copyright © 2015 John Wiley & Sons, Ltd.

Challenges in rapid soil quality assessment and opportunities presented by multivariate chemometric energy dispersive X-ray fluorescence and scattering spectroscopy

There is, especially in precision agriculture, an increasing demand world over for affordable sensors for in situ (field deployable) soil quality assessment (SQA) applicable at an ecological scale due to the interplay between soil quality and environmental degradation. Although spectrometric (particularly optical) techniques offer the opportunity to meet this demand due to their high analytical versatility, their utility in rapid SQA is limited by the complexity of the soil matrix, and the interpretation of the resulting spectra and (usually) multivariate quality assurance (i.e. SQA) data. In this paper, we examine the utility of spectrometric techniques for soil analysis and critique their applicability to rapid SQA; in particular, we appraise their potential for development towards intelligent portable SQA systems for in situ application. We then evaluate in this perspective the applicability of a new method we have recently developed namely chemometrics energy dispersive X-ray fluorescence and scattering spectrometry (EDXRFS) for SQA, emphasizing its potential for realizing rapid intelligent sensor architecture for in situ SQA. We conclude that a point of care soil sensor that infers soil properties, and intelligently modulates precision agriculture may be realized by integrating the EDXRFS spectroscopy method to a portable XRF spectrometer.

Application of a portable XRF spectrometer for classification of potash glass beads unearthed from tombs of Han Dynasty in Guangxi, China

Thirty‐seven glass beads excavated from the Han Dynasty tombs in Hepu county, Guangxi, China, were analyzed using a portable X‐ray fluorescence (PXRF) spectrometer. Reference sample Corning glass D is used to check precision and accuracy of the equipment for major and minor components. The results of inductively coupled plasma atomic emission spectroscopy and PXRF are compared to evaluate the quality of equipment for trace elements. Combined with the contents of Al2O3 and CaO, a new criterion of subgroup division for potash glass based on the levels of trace elements (Rb and Sr) is proposed. The correlations of Rb and K, Rb and Al, and Sr and Ca are discussed. It is thought that saltpeter was the main flux used to produce potash glasses of different groups. The positive correlation between Rb and Al, and Rb and K indicates that potassium aluminosilicate minerals may be used as raw minerals for potash glasses of group II. The results indicate that the levels of Rb and Sr can be very helpful in subgroup definition and provide useful clues to the raw materials used for glassmaking and provenance study of the potash glass found in Guangxi, China. Copyright © 2013 John Wiley & Sons, Ltd.

Performance of three different Si X-ray detectors for portable XRF spectrometers in cultural heritage applications

In this work, a study of detection systems in portable X-ray fluorescence (PXRF) spectrometry was performed. An assessment of various detectors and their influence on the measurement of trace elements in different bulk materials, from light to heavy matrices, was done. Four reference materials were analyzed: Orchard Leaves (NBS-1571); Bone Meal (NIST-1486); River Sediment (NBS-1645) and Free-Cutting Brass (NBS-1105). Detection limits were calculated for the elements present in the reference materials, quantitative calculations were performed for three known samples and a comparison was made for each detector. Three case studies were also performed in order to appraise the behavior of the detection systems: A paper document from 1909, a potassium alum/calcite mixture and a Portuguese coin.

Silk Road glass in Xinjiang, China: chemical compositional analysis and interpretation using a high-resolution portable XRF spectrometer

In this paper we explore the major, minor and some trace elements of sixty-five glass beads from eighteen oasis sites both north and south of the Taklamakan Desert, the ancient centre of the Silk Routes linking East and West; the samples date from the Warring States period (475–2211 BCE) to the Tang Dynasty (618–907 CE). Using a high-resolution portable XRF spectrometer, with special attention to issues of surface weathering and sample preparation, we obtained quantitative chemical compositional data that, when combined with archaeological context and the technology of bead manufacture, provide the basis for an understanding of both changes in glass type over time, and possible source areas for the Xinjiang glasses. While glass beads at the early sites (1st c. BCE to 4th c. CE) were coming primarily from Kushan-controlled territories in northern India, Pakistan and Afghanistan, with a small contribution from central China, most of the later glass (4th–10th c. CE) is similar to that produced in the Sasanian Empire at such sites as Veh Ardashir in central Iraq. These changes most likely reflect changing cultural and economic conditions in the Silk Road towns.

Sourcing ceramics with portable XRF spectrometers? A comparison with INAA using Mimbres pottery from the American Southwest

Seventy-five intact Mimbres and Jornada pottery sherds from the American Southwest were analyzed by portable XRF and instrumental neutron activation analysis (INAA). Examination of the data demonstrates that INAA and portable XRF results for elements common to both analyses can be used to construct similar compositional groups. When individual compositional groups are compared to one another, it is apparent that unambiguous separation of compositional groups is challenging by portable XRF given (1) the limited number of key discriminating elements that can be measured relative to INAA, and (2) the relative analytical precision and accuracy of portable XRF for measurements of intact heterogeneous ceramics. We conclude that sourcing intact ceramics by portable XRF is challenging and that bulk analytical measurements, such as INAA, remain a better approach for sourcing archaeological pottery.

Characterization of some ancient glass vessels fragments found in Xinjiang, China, using a portable energy dispersive XRF spectrometer

AbstractIn this article, a portable energy dispersive X‐ray fluorescence spectrometer having determination capability for elements of Na and Mg is applied to characterization of the 58 ancient glass vessels fragments found in Xinjiang, China, successfully. These ancient glass samples were found in different historical sites dated from the Han Dynasty (202 B.C.–220 A.D.) to early Yuan Dynasty (1271–1368 A.D.). The chemical composition difference between the original weathered and inner fresh surfaces is distinguished. Using Mg, Ca, Al and K as the diagnostic elements, the glass samples analyzed are mainly classified into three types through cluster analysis. Each type of glass seems to be produced under different recipes. The techniques used to make these glasses and their possible provenances are discussed briefly. The obtained results provide new useful information for further understanding of the exchange and trade networks related to early glasses found in Xinjiang, China. Copyright © 2011 John Wiley & Sons, Ltd.

A novel portable XRF spectrometer with range of detection extended to low‐Z elements

AbstractX‐ray fluorescence (XRF) analysis is one of the most widely used techniques for material analysis in the field of cultural heritage, thanks to its non‐destructive and multi‐elemental character and also to the possibility of using portable instrumentations. The need of compact systems for in situ analyses results generally in a worse, more limited performance: the detection of low‐Z elements is the most affected aspect. In this article, we present a custom‐realised portable XRF spectrometer developed in Florence at the LABEC laboratory of Istituto Nazionale di Fisica Nucleare (INFN), in collaboration with ICVBC of Consiglio Nazionale delle Ricerche (CNR). The system features a high efficiency for a wide range of elements, even at low Z (down to sodium), thanks to the use of two tubes with different anodes and to the presence of a continuous helium flow in front of the tubes and the detector, in order to enhance transmission of both primary and characteristic X‐rays. After a detailed description of the spectrometer, the experimental characterisation of its performance is presented: efficiency curves obtained from the analysis of thin standards are reported, together with minimum detection limits for some elements in a thick target of medium‐low density matrix. Examples of measurements, which demonstrate the capability and effectiveness of this spectrometer, are also reported. Copyright © 2011 John Wiley & Sons, Ltd.

탁상형 및 휴대형 X-선 형광 분석기를 이용한 폴리에틸렌 및 폴리프로필렌 시료 중 RoHS 규제 물질의 비교 분석

As a basic research for development of the domestic portable XRF spectrometer, we discussed the analytical results of bench-top and portable XRF methods for RoHS materials of the Cd, Pb, Hg, Cr(IV), polybrominated biphenyls(PBB) and polybrominated diphenyl ehters(PBDE). The instrumental parameters such as measurement time of bench-top and portable XRF were optimized using certified reference materials of polyethylene and polypropylene with 5 hazardous materials of 0~1,200 mg/kg. The quantitative analysis of total-Cr, total-Br, Cd, Hg and Pb in certified reference materials and plastic samples were compared by empirical method, fundamental parameter method of bench-top XRF and portable XRF.

Comparison of matrix effects on portable and stationary XRF spectrometers for cultural heritage samples

In this work, we compare the matrix effects for two different X-ray fluorescence spectrometers, a portable and a stationary one, in order to evaluate their performances in terms of scattering radiation for different matrices. Five reference materials were analyzed: orchard leaves (NBS-1571), clay (ISE-954), bone ash (NIST-1400), 70% copper alloy (BCR-691) and 22 ct gold alloy (Fisher). The results obtained showed similar behavior for both spectrometers. The lowest background was obtained for the light matrix and an increase was observed for intermediate atomic number matrices, reaching a maximum for copper and gold alloys. In spite of that the lowest background had been obtained for the light matrix, the portable system presents a tremendously high background when compared to the stationary one. For this matrix, some of the trace elements were almost not detected by the portable spectrometer, which makes difficult their characterization with this system. For medium Z matrices there is an increase on the Compton peak and a decrease on the Rayleigh one, reaching a similar intensity. Finally, for heavy matrices, the Compton peak almost disappears and the Rayleigh effect takes the lead. Three case studies were also performed in order to appraise the behavior of the spectrometers: a paper document from the XVIII century, a sample of archaeological bone from the Middle Ages and a Portuguese coin from the XIX century.

Change in chemical composition of early Islamic glass excavated in Raya,Sinai Peninsula, Egypt: on-site analyses using a portable X-ray fluorescence spectrometer

The Raya port (eighth to 12th centuries) on the Sinai Peninsula, Egypt, was one of the important port cities for the Red Sea trade. We performed on-site analyses of Islamic glass vessels (used in eighth to 11th centuries) mainly from this site in Egypt using a portable XRF spectrometer. The aim of this paper is to contribute to our understanding of the chemical compositions of early Islamic glass vessels by comparing their archaeological date and typology. In the early Islamic period, glass objects were mainly produced from natron as the soda source. Among the natron glass analyzed in this study, glass vessels with low titanium and iron and high strontium contents, which were probably produced in the Syria–Palestine region, were excavated in the eighth century layer. From the ninth century layer, a large number of samples with high levels of calcium, titanium and iron, probably produced in Egypt, were found. It should be noted that a large number of glass vessels with this chemical composition were found at the Raya site, because this type of glass was rarely reported from other Islamic sites. We finally concluded that this type of glass seems to be produced under a fixed recipe, although some samples contain a colorant or decolorized materials.

Archaeological analysis of Roman glass excavated from Zadar, Croatia, by a newly developed portable XRF spectrometer for glass

AbstractA newly developed portable x‐ray fluorescence spectrometer has been evaluated through the onsite and nondestructive analyses of 109 Roman glass artifacts excavated at a Roman cemetery found in Zadar, Croatia. The spectrometer has been designed for on‐site analysis of archaeological glass objects. The instrument consists of an x‐ray tube with a Pd target operated at up to 40 kV, silicon drift detector (SDD) with a polymer window, and an enlargeable vacuum sampling chamber. With this system, quantitative analysis of the light elements such as Na and Mg that are important components of glass, as well as heavy trace elements, was successfully carried out. The obtained results evidenced the use of Natron as fluxing agent with alkali contents of 14–22 wt% Na2O, 0.5 wt% MgO and 1.2 wt% Al2O3. In addition, it was found that the differences in the use of Mn and/or Sb as decolorizing agent in colorless bell‐shaped flasks collected from 10 different localities along the coast of Croatia comparing with the same type flasks excavated from Zadar. Copyright © 2009 John Wiley & Sons, Ltd.

Complementary use of the Raman and XRF techniques for non-destructive analysis of historical paint layers

The portable XRF spectrometer has been applied in situ for the non-destructive elemental mapping of the pigment components of the XV c. mural painting and frescos of the Little Christopher chamber in the Main Town Hall of Gdańsk, Poland. For a sufficiently large data collection the principal component analysis (PCA) was applied in order to associate the most intense lines of the elements Ca, Cu, Fe, Pb, and Hg in the XRF spectra with the palette of colors: white, brown, green, blue, red, yellow, and black observed in the painting. This allowed to limit the number of extractions of the micro-samples for the complementary Raman measurements thus assuring the practically non-destructive character of the entire analysis. The reliable identification of the pigment compositions was based on coincidence of the XRF, PCA and the Raman results which confirmed the presence of the chalk, malachite, azurite, red lead, mars red, mars yellow and candle black in the historical paints, except of the carbon-based black pigment being out of the XRF detection range. Different hues of the green paint were specified and the variety of the red and brown ones was ascribed to compositions of the Pb- and Fe-based red pigments (Fe 2O 3 and Pb 3O 4) with addition of the vermilion (HgS) and carbon black, in agreement with literature. The traces of elements: Ba and Sr, Sb and Mo, and also Cd, were ascribed to the impurities of Ca, those of some ochre pigments, and to the soluble Cd salts, respectively.

A portable micro-X-ray fluorescence spectrometer with polycapillary optics and vacuum chamber for archaeometric and other applications

A portable focused-beam XRF spectrometer was designed, constructed, and manufactured. The spectrometer allows to detect and perform analysis of chemical elements from Na upwards. The system is equipped with a compact vacuum chamber to reduce absorption of both the excitation and the fluorescence radiation in air. A low power Pd-anode tube operated up to 50 kV and 1 mA with a point focus of 400 μm is used as excitation source. A polycapillary lens with a spot size of about 160 μm, or a collimator with a 1 mm inner diameter can be used alternatively for either focusing or collimating the primary beam. The fluorescence radiation is collected by an Si drift detector with an active area of 10 mm 2 and equipped with an 8 μm Be entrance window. A compact vacuum chamber was designed to house the X-ray beam optics and the detector snout. The chamber is attached to the X-ray tube and can be pumped down to 0.1 mbar. A Kapton™ window of 7.5 μm thickness allows to locate the investigated spot at about 1–2 mm distance outside of the chamber, thus minimizing absorption losses in the excitation and X-ray fluorescence radiation paths. Two lasers pointers are mounted inside the chamber. The laser beams cross at a point outside the chamber in front of the entrance window and coincide with the focal spot of the polycapillary. This paper reports some preliminary results obtained from an in situ analysis of bronze samples as well as a comparison of these data with those given by other laboratory spectrometers and the reference values provided by the Italian bronze foundry Venturi Arte Bologna, Italy.

Application of a Portable XRF Spectrometer for the Non‐Invasive analysis of Museum Metal Artefacts

The present paper reviews examples of the application of a portable - in house developed- XRF spectrometer for the analysis of museum metal artefacts in Greece. Specific topics are addressed, in particular, to which extent the qualitative or quantitative XRF analyses reveal important information about the raw materials and manufacture techniques used for gold, silver and bronze alloys in antiquity. The analytical information that it is gained by means of the XRF measurements is further assessed in comparison with the existing archaeometallurgical knowledge.

Quantitative elemental analysis of Della Robbia glazes with a portable XRF spectrometer and its comparison to PIXE methods

A portable XRF spectrometer has been developed at the Centre de Recherche et de Restauration des Musees de France (C2RMF), in Paris. The instrument has been successfully used on many occasions to analyse qualitatively various important works of art. In the present study, it has been utilised for the analysis of two glazed sculptures located in the cathedral of Seville (Spain) and attributed to the Della Robbia workshop. The aim was to perform a quantitative analysis in order to determine the elemental composition of the glazes. The results are compared with those previously obtained with particle induced x-ray emission (PIXE) and µ-PIXE techniques at the C2RMF on other Della Robbia wares located at the Louvre museum. The data provide information on the two sculptures, which is discussed in relation with what is known on the Florentine production at the Renaissance. Copyright © 2006 John Wiley & Sons, Ltd.

Complementary use of PIXE-alpha and XRF portable systems for the non-destructive and in situ characterization of gemstones in museums

Gemstones on gold Hellenistic (late 4th century BC, 1st AD) jewelry, exhibited at the Benaki Museum of Athens, were analyzed in situ by means of two non-destructive and portable analytical techniques. The composition of major and minor elements was determined using a new portable PIXE-alpha spectrometer. The analytical features of this spectrometer allow the determination of matrix elements from Na to Zn through the K-lines and the determination of higher atomic number elements via the L- or M-lines. The red stones analyzed were revealed as red garnets, displaying a compositional range from Mg-rich garnet to Fe-rich garnet. The complementary use of a portable XRF spectrometer provided additional information on some trace elements (Cr and Y), which are considered to be important for the chemical separation between different garnet groups. A comparison of our results with recent literature data offers useful indications about the possible geographical provenance of the stones. The analytical techniques, their complementarity and the results obtained are presented and discussed.

A new portable XRF spectrometer with beam stability control

AbstractA new portable XRF spectrometer which allows control of the energy and the intensity stability of the emitted x‐ray beam has been designed and built. The control is obtained by measuring the x‐ray fluorescence generated by a double Ag/Ba thin target when crossed by the x‐ray beam during a measurement. The silver and barium fluorescence K lines are detected by an ancillary Si‐PIN detector and analysed by software developed at the LNS/INFN laboratories. The new portable spectrometer, the beam stability control method, the evaluation of the system and some quantitative applications of interest in the cultural heritage field are presented and discussed. Copyright © 2004 John Wiley & Sons, Ltd.

Fluorescence from the collimator in Si-PIN and Si-drift detectors: problems and solutions for the XRF analysis of archaeological and historical materials

The investigation of archaeological and historical materials is one of the most successful applications of portable XRF spectrometers; depending on the situation, instruments with detection limits of a hundred ppm or less may be desirable. One of the technical solutions to achieve this goal still remains working with X-ray tubes at a relatively high voltage and current, i.e. 60 kV and at least 1 mA, which allows to take advantage from both an intense primary beam and the possibility of resolving such important elements as Ag, Cd, In, Sn and Sb. An Amptek SiPIN mod. XR100T and a Ketek Si-drift 5 mm 2 were tested with respect to the suitability to work in such “extreme” conditions. Both detectors show spurious lines due to the fluorescence from the collimator’s material: in order to account for these spectral contaminations and analyse samples containing the same element as the collimator, a correction method was developed and tested; this also included the evaluation of the detection limit for the collimator’s element actually contained in the sample; in our experimental conditions, the detection limit for zirconium is about 130 ppm. Though developed for the analysis of obsidians with Si-drift detectors, the method is quite general and can be applied to any collimator material.