Wavelength Dispersive X-ray Fluorescence Spectrometer Research Articles

A review of laboratory, commercially available, and facility based wavelength dispersive X-ray fluorescence spectrometers

Wavelength dispersive X-ray fluorescence (WD-XRF) spectroscopy is a widely used instrumental spectroscopy method for a variety of samples.

Effect of particle size analysis on the physicochemical characterization of Malaysian monazite

Rare earth elements (REEs) are the elements that have become extremely important to our world of technology owing to their unique physical and chemical properties, and widely used in advanced technology. Monazite is one of the mineral phosphate that contain a high amount of REEs including thorium and a small amount of uranium. In Malaysia, monazite is exist as by-product (‘amang’) from tin mining originated from Ipoh, Perak. The objective of this study is to determine the effects of the different particles size of raw and ground (milled) monazite on the physicochemical properties. The effectiveness of extraction and separation process of monazite was affected by the size of the particle. Based on the particle size distribution analysis, all the monazite samples were found to be present in the size range of 11-190 μm. The morphological and elemental composition of the monazite mineral have been characterized by field emission scanning electron microscope (FESEM) integrated with energy dispersive X-ray spectrometer (EDX). The FESEM micrographs of the monazite showed an irregular spherical structures with different sizes. The chemical composition and the mineral phases present in monazite were studied by wavelength-dispersive X-ray fluorescence spectrometer (WD-XRF) and X-ray diffraction (XRD). The XRF analysis confirmed the presence of the major REEs such as Ce, La and Nd elements in the mineral. XRD analysis also identified (Ce, La, Nd and Th)PO4 as the major phases along with quartz as minor phase. According to the FESEM-EDX and XRF analysis, smaller particle size of monazite gave higher content of REEs compare to raw monazite.

Rapid method of arsenic estimation in geological samples by WD-XRF using a novel concept of As-Pb concentration equivalence.

The presence of arsenic in ground waters of many countries has been a subject of global concern due to its toxicity. Primary sources of arsenic are geogenic, i.e. weathering and erosion of rocks and soils containing arsenic. This paper presents a rapid method for determination of arsenic in solid geological samples by wavelength dispersive X-ray fluorescence spectrometer. To achieve the best LLD (lower limit of detection), the most intense X-ray fluorescence line Kα1,2 is preferably used for determination of elemental concentrations because it pertains to the most probable transition. But the greatest challenge in arsenic estimation is the serious line overlap of AsKα1,2 lines with the equi-energy PbLα1,2 lines. By using the conventional line overlap correction methods, uncertainty and detection limits in arsenic determination are degraded to an unacceptable degree in samples which contains high lead and low arsenic concentrations. The proposed method bypassesthe line overlap issue in employing a novel concept of arsenic-lead concentration equivalence factor for the cumulative peak of AsKα1,2 and PbLα1,2 fluorescence lines. The constancy of this factor for all geological matrices facilitates arsenic determination in samples universally irrespective of matrix elements. For the method validation, 22 international certified reference materials have been analysed and the results proved to be propitious wherein only one value out of 22 determinations showed relative error more than 20% of the certified values. This attests to the high accuracy of the proposed method which can effectively determine arsenic below 5mg/kg in the presence of high lead concentration up to 1000mg/kg.

Determination of bromine, iodine, and other components in northern Hainan island soil

The emergence of the integrated wavelength-dispersive and energy-dispersive Zetium X-ray fluorescence spectrometer technique offered new chances to analyze elemental distribution with minimal sample preparation in complex matrix geological samples-northern Hainan island soils. Wavelength-dispersive X-ray fluorescence was applied for the measurement of bromine in the northern Hainan island soil. To reduce the fluctuations of the low-bromine-content measurement results, a two-channel measurement of bromine was designed, and the average value of the two-channel measurements was used as the final result. The soil samples in northern Hainan Island were rich in iodine, with a content range of a few µg/g to more than 100 µg/g, and these were particularly suitable to be analyzed by energy-dispersive X-ray fluorescence spectrometer. The geological samples in northern Hainan Island were brown, purple, and brown-red soil containing kaolinite, ilmenite, rutile, anatase, and goethite. These soil samples were rich in titanium, aluminum, and iron. The titanium concentration in the northern Hainan Island soil was anomalously high (up to 15.05%), far exceeding the content range of the calibration curve. Owing to the empirical coefficient matrix correction method, unreliable or even unreasonable results were obtained for some elements. By systematically mitigating matrix effects through the development of custom reference materials and building matrix-matched measurement and calibration routines, the quantification of Vanadium, Barium, and major components in northern Hainan Island soil samples was optimized. The efficacy of the X-ray fluorescence spectrometer method was confirmed by comparison with inductively coupled plasma–optical emission spectroscopy analysis. This work demonstrates the capability of the integrated wavelength-dispersive and energy-dispersive Zetium X-ray fluorescence spectrometer technique for reliable quantitative elemental analysis of complex matrix geological samples.

Elemental Composition and Sources of Fine Particulate Matter (PM2.5) in Delhi, India.

In this study we have analysed the elemental composition of fine particulate matter (PM2.5) to examine the seasonal changes and sources of the elements in Delhi, India from January, 2017 to December, 2021. During the entire sampling period, 19 elements (Al, Fe, Ti, Cu, Zn, Cr, Ni, As, Mo, Cl, P, S, K, Pb, Na, Mg, Ca, Mn, and Br) of PM2.5 were identified by Wavelength Dispersive X-ray Fluorescence Spectrometer. The higher annual mean concentrations of S (2.29µg m-3), Cl (2.26µg m-3), K (2.05µg m-3), Ca (0.96µg m-3) and Fe (0.93µg m-3) were recorded during post-monsoon season followed by Zn > Pb > Al > Na > Cu > Ti > As > Cr > Mo > Br > Mg > Ni > Mn > and P. The annual mean concentrations of elemental composition of PM2.5 accounted for 10% of PM2.5 (pooled estimate of 5 year). Principal Component Analysis (PCA) identified the five main sources [crustal/soil/road dust, combustion (BB + FFC), vehicular emissions (VE), industrial emissions (IE) and mixed source (Ti, Cr and Mo rich-source)] of PM2.5 in Delhi, India.

Remediation and characterization of emerging and environmental pollutants from residential wastewater using a nature-based system.

The nature-based systems (NBS) are nature inspired, unflagging, efficient, and budget friendly ideas that evolved as ideal technologies for wastewater treatment. The present study deals with the purification of residential wastewater through the NBS, covering three seasons. The NBS embedded with the Canna lily effectively eliminated organic matter, nutrients, and heavy metals. Nearly 57.2-75.2% COD, 69.9-83.2% BOD, 73.4-90.6% TSS, 51.1-71.6% PO43--P, 66.3-84.8% NH4+-N, 52-61.5% NO3--N, and 68-70.6% NO2--N removal were achieved. Heavy metals like Al, Cr, Mn, Fe, Ni, Cu, Zn, Mo, and Pb were removed, with a 98.25% reduction in the total bacterial count. The pollutant removal's kinetics was calculated using first-order kinetics. The mass removal rate of BOD was high in monsoon (22.3g/m2/d), and COD was high in summer (36.4g/m2/d). Organic compound removal (65.2%), including emerging pollutants, was observed by gas chromatography-mass spectrometry (GCMS) analysis of water and Canna samples. Wavelength dispersive X-ray fluorescence spectrometer (WDXRF) studied the elements and oxides retention by media and accumulation by the plant. The CHN content of the Canna and its morphological study was checked using the carbon CHNS analyzer and scanning electron microscope-energy dispersive X-ray (SEM-EDX), respectively. The performance of the NBS was validated using variance, correlation, and principal component analysis (PCA). This study shows the NBS effects on the remediation of environmental and emerging contaminants from residential wastewater and further use it for horticultural activities, thereby achieving sustainable development goals.

Position dispersive X-ray fluorescence

A novel scanning-free wavelength dispersive X-ray fluorescence spectrometer has been developed by combining low power X-ray tubes with X-ray optics. The X-rays are focused to a single point on the sample and then dispersed onto a flat diffracting crystal where they are spread depending on their energy through Bragg's law of diffraction onto a silicon strip detector. Throughout this study, the proposed method is referred to as Position Dispersive X-ray Fluorescence (PDXRF). The X-ray emission spectra of vanadium and copper as well as, CuO, CuS2 and V2O5 were measured. In the spectrometer energy resolutions of 3.14 eV and 8.94 eV FWHM were measured for V and Cu when measuring over a range of 4.8–5.8 keV and 6.2–9.1 keV respectively. The Kβ line shapes were fitted with a series of Voigt profiles and the energies and intensities of the Kβ valence transition peak, Kβ2,5, were determined. There was also sufficient variation in the intensity ratio of Kβ2,5/Kβ1,3 that the oxygen and sulphur compounds of V and Cu could be successfully observed and measured. The result demonstrates that this experimental setup is capable of measuring the Kβ line shape at resolutions of a few eV, allowing for chemical state analysis to be performed on 3d transition metals and their compounds such as the measurement of redox reactions to aid in battery development.

Focus on photonics, spectroscopy, and spectrometry

Optical spectrum analyzerSection:ChooseTop of pageOptical spectrum analyzer <<UV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... The FTE-8100-C optical spectrum analyzer (OSA) from Terahertz Technologies is one of the most cost-effective mini-OSAs on the market, according to the company. The full-featured instrument offers such functions as “power tilt” for dense wavelength division multiplexing channel equalization, “gain tilt” to adjust erbium-doped fiber-amplifier gain flatness, and file-based user configurations. The rugged unit is available with up to 98 channels in the C band with 50 GHz or 100 GHz channel spacing. Its touch screen and twice-a-second scan capability make it fast and simple to use. The one-button auto-test feature and full set of selectable scale limits and thresholds let users easily zero in on channel measurements. For flexibility, the channel numbers are selected in wavelength or frequency. Users can set pass/fail thresholds and store up to 1000 tests that can be downloaded via the USB PC port. Terahertz Technologies Inc, 169 Clear Rd, Oriskany, NY 13424, www.teratec.us UV Raman spectrometerSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometer <<Monochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... Wasatch Photonics has added a compact, cost-effective UV Raman spectrometer to its family of modular Raman spectroscopy products for research and industry. The use of UV excitation makes the WP 248 suitable for fluorescence-free Raman and UV resonance Raman (UVRR) spectroscopy to enhance sensitivity and selectivity. Applications include gas detection, materials analysis, and UVRR studies of structure and dynamics in biomolecules such as proteins and nucleic acids. The stand-alone WP 248 covers a 400–3200 cm−1 range with 14 cm−1 resolution and uses a UV-enhanced CCD for detection. It offers free space input and an f/2.0 numerical aperture for superior signal collection and high-throughput detection. Designed for use with a compact 248.6 nm neon–copper laser, it comes with a triggering cable to synchronize acquisition with the laser. Wasatch Photonics, 808 Aviation Pkwy, Ste 1400, Morrisville, NC 27560, https://wasatchphotonics.com Monochromator for UV spectroscopySection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec... <<Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... McPherson has upgraded its compact model 234/302 monochromator for UV spectroscopy: The internal surfaces now have an optimized ultrablack low-scatter finish, the range of masterpiece gratings has been expanded, and spectrograph accessories and an improved turret are available. The enhancements improve efficiency and spectral resolution from the deep UV and vacuum UV (VUV) to the visible and near-IR. The model 234/302 can be equipped with a grating turret that allows users to broaden the accessible wavelength range without breaking vacuum or purge. With a digital grating drive for precise wavelength selection and positioning, the compact VUV spectrometer is easy to use as a scanning monochromator or as a spectrograph with a microchannel plate intensifier or a CCD detector. McPherson Inc, 7A Stuart Rd, Chelmsford, MA 01824, https://mcphersoninc.com Near-IR Raman spectrometerSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete... <<Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... Optimized for performance in the near-IR region, the TPIR-785 Raman spectrometer from Teledyne Princeton Instruments has ultrahigh sensitivity and is suitable for use in such areas as biological, medical, and life sciences research. The system uses an f/2 spectrograph with lens optics designed to provide high light throughput and imaging quality. Users can tailor the instrument’s performance for an optimal spectral resolution up to 5 cm−1 or an optimal spectral range up to 80–3650 cm−1. The system includes a 785 nm Raman probe, a universal fiber adapter, a manual adjustable slit, and a high-power, temperature-stabilized 785 nm laser. A proprietary CCD delivers near-IR quantum efficiency greater than 70% at 1000 nm. The “super-deep-depletion” sensor has a 1340 × 400 array composed of 20 µm2 pixels. It can be thermoelectrically cooled to −90 °C for ultralow dark current, which allows integration times from 10 µs to hours. The detector provides spectral rates higher than 1 kHz, offers readout speeds up to 16 MHz, and uses two readout ports. Teledyne Princeton Instruments, 3660 Quakerbridge Rd, Trenton, NJ 08619, www.princetoninstruments.com Shortwave-IR laserSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laser <<Positioning stage for pho...Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... Beyond Photonics has launched its compact piezo-tunable Swift single-frequency short-wave IR (SWIR) laser. The rugged, solid-state laser is suitable for lidar and laser spectroscopy applications that require very stable high-power reference and seed lasers. It is initially offered in the range of 2050 nm, but it can be adapted to many other near- and shortwave-IR wavelengths. The Swift is optimized for use in coherent and direct-detection eye-safe lidar systems or other SWIR applications that require ultralow short-term frequency stability and broad, fast tunability. With its high CW output power—greater than 35 mW standard and up to 100 mW optional—and less than 10 kHz/ms short-term frequency jitter, the Swift is suitable for use as a master and local oscillator source in lidar systems. Fast and broad mode-hop-free frequency tuning enables next-generation spectroscopic applications, such as pollution monitoring and greenhouse gas measurements that use differential absorption lidar techniques. Beyond Photonics LLC, 6205 Lookout Rd, Ste B, Boulder, CO 80301, www.beyondphotonics.com Positioning stage for photonic applicationsSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho... <<Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... Physik Instrumente (PI) now offers a compact, modular, five-axis stage with closed-loop motors for precision alignment and positioning of photonics and optics components, such as fibers, waveguides, and lenses. The F-122 5DOF stage consists of a three-axis linear module with linear encoders for direct position measurement and PI’s WT-85 and WT-100 goniometers. The goniometers are combined with a shared pivot point to perform high-precision angular motion with resolution to 3.5 µrad. Submicron precision is ensured by highly accurate mechanical components and encoder feedback for closed-loop operation. A multiaxis controller and software with automated alignment functionality are available. With programming interfaces, including LabVIEW and MATLAB, users can integrate a PI controller into their own programs. Physik Instrumente LP, 16 Albert St, Auburn, MA 01501, www.pi-usa.us Spectrophotometer for turbid mediaSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur... <<Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... The novel SphereSpectro 150H system from Gigahertz-Optik simultaneously discriminates and quantifies both the spectral absorption coefficient and the spectral effective scattering coefficient of scattering media. The spectrophotometer uses an integrating sphere to measure the total reflected and transmitted light of an illuminated sample. From those two quantities, the absorption coefficient and the effective scattering coefficient are calculated based on the radiative transfer equation. The SphereSpectro 150H covers the wavelength range between 200 nm and 2150 nm, with modular versions available for subranges within that spectral range. The compact tabletop device offers fast, precise, and absolute measurements; simple operation; and a large sample chamber with an optimized sample holder. Applications include materials analysis, biophotonics, and quality assurance. Gigahertz-Optik Inc, Boston North Technology Park, Bldg B, Ste 205, Amesbury, MA 01913, https://light-measurement.com Compact Q-switched laserSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur...Compact Q-switched laser <<Multispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... Hübner Photonics has introduced the Cobolt Tor XE compact Q-switched laser at 1064 nm and with 0.5 mJ/pulse. It delivers short pulse lengths of less than 3.5 ns at kHz repetition rates and high pulse-to-pulse stability—jitter is less than 2 μs—in a TEM00 beam. The advanced, integrated control electronics use external or internal signals to trigger the emission from single pulses up to 1 kHz pulse trains or bursts of pulses. The Cobolt Tor XE is manufactured using proprietary HTCure technology; according to the company, the resulting hermetically sealed package improves the laser’s reliability under varying environmental conditions. It can be used in laser marking, laser-induced breakdown spectroscopy, micromachining, and photoacoustic microscopy applications. Hübner Photonics Inc, 2635 N 1st St, Ste 202, San Jose, CA 95124, https://hubner-photonics.com Multispectral in vivo IR imagingSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ... <<Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... According to Photon Etc, its IR VIVO preclinical imager provides noninvasive spectral imaging in the first (NIR) and second (NIR-II) biological windows, from 900 nm to 1620 nm. It combines micron-scale spatial resolution, real-time imaging, and full multispectral coverage for in vivo research on small animals or other living organisms. With fast acquisition speed, multicolor imaging, and good penetration depth—10 times as great as traditional visible optical systems, the company claims—the IR VIVO captures both structure and function. Because it uses near- and shortwave-IR, the imager benefits from reduced scattering and minimal tissue absorption and autofluorescence, which allows deeper, clearer imaging than can be achieved with standard optical systems. Emission of several fluorophores can be isolated with a high-efficiency tunable filter and ultralow-noise scientific-grade indium gallium arsenide camera. Photon Etc, 5795 Ave de Gaspé, #222, Montreal, QC H2S 2X3, Canada, http://photonetc.com Tube-below WDXRF spectrometerSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom... <<High-speed cameraProgrammable IR spectrome... Due to its tube-below optics, the ZSX Primus IVi wavelength-dispersive x-ray fluorescence (WDXRF) spectrometer from Rigaku optimizes the measurement of typical gravity-loaded samples such as liquids and analyzes alloys and plated metals. According to the company, the new model improves on previous systems by having the smallest footprint in its class and an efficient new drive sequence that decreases the time between multiple high-speed, precision measurements. It includes new sample film corrections, and a redesigned control system optimizes movement sequences. The ZSX Primus IVi spectrometer has a patented vacuum partition system for analyzing liquids. Because the spectroscopic chamber is separated from the sample chamber when the helium gas is being changed, the conversion from vacuum to helium atmosphere can be completed in less than 2 minutes. Rigaku Americas Corporation, 9009 New Trails Dr, The Woodlands, TX 77381-5208, www.rigaku.com High-speed cameraSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed camera <<Programmable IR spectrome... According to Vision Research, its Phantom T1340 high-resolution camera doubles the capabilities of other 4 MP cameras in its class. It captures images up to 13 GP/s. Its 2048 × 1952 pixel low-noise sensor and compact size make the camera suitable for demanding measurement applications such as object tracking, flow visualization, and microscopy and for modern imaging techniques such as digital image correlation. A binned mode provides higher throughput and a sensitivity boost at 1 MP and below. Because the T1340 includes Phantom CineMag V compatibility for an ultrafast, secure workflow and for direct recording of long-duration events, the camera can be used in outdoor environments. A 10 GB ethernet option is available for fast file downloads, so users can continue shooting with reduced downtime. Vision Research Inc, 100 Dey Rd, Wayne, NJ 07470, www.phantomhighspeed.com Programmable IR spectrometerSection:ChooseTop of pageOptical spectrum analyzerUV Raman spectrometerMonochromator for UV spec...Near-IR Raman spectromete...Shortwave-IR laserPositioning stage for pho...Spectrophotometer for tur...Compact Q-switched laserMultispectral in vivo IR ...Tube-below WDXRF spectrom...High-speed cameraProgrammable IR spectrome... << The PEAK XNIR, a novel high-throughput OEM spectrometer from Ibsen Photonics, combines Ibsen’s high-efficiency fused-silica transmission gratings with DLP Pico technology from Texas Instruments. It provides a dimension of spectral programmability that, according to the company, has not been possible with other available spectrometer technology: Users can control the relative power and exposure time independently for each wavelength in a spectrum. The PEAK XNIR’s retroreflective advanced optical design allows for a compact form factor with high resolution, sensitivity, and environmental ruggedness. It features a wavelength range of 1650–2400 nm, 10 nm resolution, and a high numerical aperture of 0.22. The PEAK XNIR is suitable for process analytical technology because it offers real-time in-line monitoring and measurements for near-IR spectroscopy. Ibsen Photonics A/S, Ryttermarken 17, DK-3520 Farum, Denmark, https://ibsen.com © 2021 American Institute of Physics.

Bolu’da Ev Tozu ile İlişkili Sağlık Risklerinin Tahmin Edilmesi

The levels of metals associated with dust is higher in indoor environment as compared to settled dust or soil in the exterior counterpart in the urban centers. The metals can be transferred to human body via inhalation, ingestion and dermal contact upon exposure and pose a significant health problem. The primary objectives of this study are (i) to determine the levels of metals in home dust samples in Bolu, Turkey, (ii) to assess the associated health risk when citizens are exposed to these metals in indoor environment. To end this, sixteen vacuum cleaning bags containing dust were collected from the homes located in the city center of Bolu (Turkey) between November and December 2017. The collected samples were analyzed by employing Wavelength Dispersive X-Ray Fluorescence (WDXRF) spectrometer in terms of major (Al, Ca, Cl, K, Mg, Na, P, S and Si) and minor (As, Ba, Br, Ce, Co, Cr, Cu, Fe, Mn, Nb, Ni, Pb, Rb, Sn, Sr, Ti, Y, Zn and Zr) metals at Turkish Atomic Energy Agency, Radiation and Accelerator Technologies Department, Ankara (Turkey). The measured levels of metals in the samples were ranged from 6.52±1.60 µg g-1 for Y to 10.4±3.3 % for Na. The crustal enrichment factor (EFcrust) was calculated in order to understand the contamination level of household dust samples as compared to soil composition. EFcrust results revealed that there is minimal enrichment of Si, Rb, Ti, Ba, K, Y and Mn in household dust samples with respect to soil composition. On the other hand, Zn, Cl, and S found to be extremely enriched in the samples according to EFcrust values. Health risk assessment due to household dust metal exposure depicted that ingestion of dust particles is the main route of exposure for both adults and children. Overall, the calculated HQ value &amp;lt;1.0 suggesting there is no significant non-carcinogenic health risk for the residents. Cancer risks associated with Pb and Cr were estimated to be within the EPA’s safe limits (1x10-6 and 1.0x10-4).

Chemical effect on Lγ4 and Lγ5 X-ray lines in Thallium complexes

The previous outcomes of Wavelength Dispersive X-ray Fluorescence (WDXRF) technique were strictly restricted to the compositions of varieties of the materials where non-destructive and non-intrusive features can be persecuted. At present, the advancement in WDXRF spectrometer has made a huge impact on the chemical profiles in distinct chemical materials. The present work offers useful insights regarding the chemical effect in various Tl complexes viz., Tl pure, Tl(NO3)3, Tl2O3, TlI, TlCl and Tl2SO4 on the Lγ4 and Lγ5 X-ray lines. To our best knowledge, the data associated with the Lγ4 and Lγ5 X-ray lines of Tl complexes were not reported in the literature. The obtained findings indicate that the Lγ4 X-ray line emitted from different Tl complexes exhibit energy shift ~ (4–7.21) eV while the Lγ5 X-ray line shows ~ (1.4–4.4) eV with respect to that emitted from the pure Tl. In general, the Tl+3 complexes show large energy shifts and relative intensity ratios as compared to the Tl+1 complexes for both X-ray lines. The sharply diverging profile changes observed in different Tl complexes can be understood in terms of the mixed-valence states, relative intensity ratio, effective charge, core-valence exchange interactions, crystal effect and distinct ligands. Additionally, the possible correlation between energy shifts and factors affecting these are also examined in the present work.

Source Identification of Trace Elements in PM2.5 at a Rural Site in the North China Plain

An intensive sampling of PM2.5 was conducted at a rural site (Gucheng) in the North China Plain from 22 October to 23 November 2016. A total of 25 elements (Al, Na, Cl, Mg, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Sr, Cd, Ba, Pb, and Sb) from PM2.5 filter samples collected daily were measured using a wavelength dispersive X-ray fluorescence spectrometer. Cl, S, and K were the most abundant elements, with average concentrations of 2077.66 ng m−3 (range 118.88–4638.96 ng m−3), 1748.78 ng m−3 (range 276.67–4335.59 ng m−3), and 1287.07 ng m−3 (range 254.90–2748.63 ng m−3), respectively. Among noncrustal trace metal elements, the concentration of Zn was the highest, with an average of 397.74 ng m−3 (range 36.45–1602.96 ng m−3), followed by Sb and Pb, on average, of 299.20 ng m−3 and 184.52 ng m−3, respectively. The morphologies of PM2.5 samples were observed using scanning electron microscopy. The shape of the particles was predominantly spherical, chain-like, and irregular. Positive matrix factorization analysis revealed that soil dust, following by industry, secondary formation, vehicle emissions, biomass and waste burning, and coal combustion, were the main sources of PM2.5. The results of cluster, potential source contribution function, and concentration weighted trajectory analyses suggested that local emissions from Hebei Province, as well as regional transport from Beijing, Tianjin, Shandong, and Shanxi Province, and long-range transport from Inner Mongolia, were the main contributors to PM2.5 pollution.

Evaluation of Analytical Precision of Polychromatic Simultaneous WDXRF Spectrometer and Application to Valence Analysis of Cathode Materials of Lithium-Ion Batteries.

A polychromatic simultaneous wavelength-dispersive X-ray fluorescence (PS-WDXRF) spectrometer can measure the valence changes of 3d transition metals with high precision in the laboratory. Adjustment and maintenance of the drive mechanism are unnecessary, and high-precision measurements are possible in a short time because the optical system has no moving parts and is compact. We have developed a PS-WDXRF spectrometer with improved analytical precision that can measure simultaneously the valence changes of three main elements, Mn, Co, and Ni, which are used as cathode materials in Li-ion batteries (LIBs). In this study, the analytical precision of the spectrometer is evaluated, and its precision is confirmed with actual battery cathodes. The identification precision of the fluorescent X-ray peak energy is <0.015 eV, and the valence identification precision is obtained to be <0.06. LiNi0.5Co0.2Mn0.3O2 (NCM523)-based LIB cathodes are analyzed under conditions maintaining this precision, and the valence changes of the 3d transition metals in NCM523 during charging and discharging are found to be 0.68 for Ni, 0.19 for Co, and 0.08 for Mn. These results indicate that Ni contributes the most to the redox process in NCM523-based LIBs, Co contributes slightly, and Mn does not contribute.

Application of handheld X-ray fluorescence spectrometer for major element analysis and characterization of geological samples in Southern Thailand

The handheld X-ray fluorescence spectrometer (hXRF) was applied to major element analysis in the geological samples and the results were compared with the results of the wavelength dispersive X-ray fluorescence spectrometer (WDXRF). In addition, the analytical compositions were confirmed by X-ray diffractometer (XRD) and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX). In the case of pXRF analysis, eight geological reference materials were used to calibrate the analytical method and four known concentration samples were used to prove the method. In research, ten geological samples from Phuket province, Thailand were collected with different depths corresponding to O horizon (0-0.1 m), A horizon (0.1-0.3 m), B1 horizon (0.3-1.0 m), B2 horizon (1.0-2.0 m), C1 horizon (2.0-3.0 m), C2A horizon (3.0-5.0 m), C2B horizon (5.0-8.0 m), C3 horizon (8.0-12.0 m), D horizon (12.0-20.0 m) and RK horizon (> 20.0 m). The elemental analysis results showed that the pXRF results were matched well with that WDXRF results. The concentration range in ten samples were Si (18-22 wt%), Al (12-15 wt%), Fe (1-4 wt%), K (0.4-3.2 wt%) and Ti (0.2-0.4 wt%). The concentration of some elements such as Ca and Mg on those ten samples are low and they are unable to analysed by hXRF. The XRD patterns revealed that all samples consisted of quartz, kaolinite, halloysite, illite, vermiculite and biotite.

Determination of iron and sulfur valence state in coal ashes by wavelength-dispersive X-ray fluorescence spectrometric technique

This paper describes the technique developed for X-ray fluorescence determination of sulfur and iron valence state in coal concentrates and ashes. The X-ray emission spectra of iron and sulfur were measured using the wavelength-dispersive X-ray fluorescence spectrometer. Samples were prepared as pressed powder pellets on a boric acid substrate. To estimate sulfur valence state SKβ’ satellite was employed. Obtained data show that certified reference material ZUK-2 contains mainly sulfate sulfur and certified reference material KMM-1 contains mainly sulfide sulfur. Results of X-ray fluorescence analysis correspond to certified mineral composition and were proved by the results of certified gravimetric technique analysis. The ratio of divalent and total iron contents was measured using the ratios of FeKβ5 line and FeKβ’ satellite intensities to FeKβ1,3 line intensity. The calibration plots were constructed using certified reference materials of coal concentrates and ashes. The FeO content was determined in CRMs SO-1 (Russia) and CTA-FFA (Poland) for the first time. The accuracy was estimated by comparison with certified titrimetric method results. Using the FeKβ5 and FeKβ1,3 lines intensities ratio allows to quantify ferrous iron.

Assessment of Vegetables and Soils from Minjingu Village-Tanzania using WDXRF Technique

Wavelength dispersive x-ray fluorescence (WDXRF) spectrometer was used to analyze heavy metal concentration in soils and vegetables. The soil and vegetable samples were randomly collected from Minjingu village of Manyara region in Tanzania. The results indicate the soils to be contaminated with heavy metals with mean concentrations of 53±0.4 For Mn, 40±0.2 for Sr, 2059±4.2 for Fe, 760±2.7 for Al, 12±0.3 for Cs and 4±0.04 for Ni in mg/kg which was above the Maximum Tolerable Limits (MTLs). Except Cl was below MDL. While vegetables recorded the mean concentrations of 60±1.2 for Mn, 68±0.1 for Sr, 620±2.36 for Fe, 284±1,13 for Al, 56±0.5 for Cs, 13±0.1 for Ni and 714±0.7 for Cl in mg/kg. The reference and experimental results of soil and vegetables revealed that the optimized machine has given the best results, where the experimental data was very close to the reference values The reference material of soil 7 and International Atomic Energy Agency (IAEA) 395 for vegetables shows the deviation of less than 2%.The Minimum Detection Limit (MDL) for vegetables and soil of the WDXRF spectrometer was obtained under low back ground for different matrix effects. There were high correlation coefficient of heavy metals in soils and vegetables at 99% level. The findings indicate that Minjingu soils and grown vegetables were highly contaminated with heavy metals mainly from soils and polluted air, at levels able to pose detrimental health effects to the consumers. Thus need of regular monitoring of the grown vegetables around phosphate mines is recommended.

In-House Valence Evaluation of Cathode Active Materials in Lithium-Ion Batteries

In the development of lithium-ion batteries (LIBs), cathode materials are being further improved to achieve not only higher energy capacity but also longer cycle life. Analyzing the valence of the cathode active materials during charge and discharge cycles is one of the practical methods to understand the redox mechanism and degradation mechanism, which can help in achieving higher energy capacity and longer life. The valence has been evaluated using X-ray absorption fine structure (XAFS) measurements with a synchrotron X-ray source. To conduct in-house analyses of valence, we developed a polychromatic simultaneous wavelength dispersive X-ray fluorescence (PS-WDXRF) spectrometer, which is comprising an X-ray tube, a slit, a flat analyzing crystal, and a silicon strip detector (SSD) [1]. The X-ray dispersed by the crystal is simultaneously detected by the SSD, and the detected signals at each channel provide intensity information at corresponding energy. Because there are no moving parts in the optical setup, the spectrometer is possible to detect the chemical changes, including valence changes, of 3d transition metals with high precision. Two PS-WDXRF spectrometers were developed. One spectrometer comprises a 1280-channel SSD and a Ge (220) crystal to detect X-rays in the range around 5.38 - 6.52 keV, which is designed for manganese. Another spectrometer comprises same components with another one and the range of detecting X-ray energy is 6.27 – 7.89 keV, which is designed for cobalt and nickel. The first step was to obtain and analyze data of pressed powders of manganese oxides using the spectrometer for manganese. Thus, powders of MnO (II), Mn2O3 (III), MnO2 (IV), and KMnO4 (VII) were placed in the evacuated chamber of the experimental setup. An X-ray tube voltage of 20 kV and a current of 100 mA was applied, and the target was made from Rh and no filter was used. A 5-min measurement was repeated five times for each sample. The PS-WDXRF analysis showed that the specimens achieved clearly different peak energies which belong to more fine electron transition fluorescence lines. This means that the WDXRF has sufficient energy resolution, and the valence information is obtained by the peak energy shift derived from the chemical shift [2, 3]. The second step was to obtain and analyze data of pressed powders of cobalt oxides and nickel oxides using the spectrometer for cobalt and nickel. Thus, powders of CoO(II), LiCoO2(III), NiO(II) and LiNiO2(III) were placed in the evacuated chamber of the experimental setup. An X-ray tube voltage of 20kV and a current of 100 mA was applied, and the target was made from W and no filter was used. This experiment demonstrated the discriminability of fluorescence peak energy shift derived from the chemical shift, in spite of the worse channel resolution. These results indicate that there is a potential for valence evaluation of cathode materials in a short time with highly precise energy resolution. These spectrometers were applied to the evaluation of actual cathode active materials in LIBs which is including manganese, cobalt or nickel. Some different states of cathode materials were prepared and the valence estimation was performed using the PS-WDXRF spectrometers. The relationship between the valence result and state of charge/discharge was confirmed, which shows that the valence number of LIBs cathode material is in accordance with the reaction formula. The recent results of valence evaluation on actual cathode active materials in LIBs will be presented in detail. [1] K. Sato, A. Nishimura, M. Kaino, S. Adachi, X-Ray Spectrom. 46, 330–335 (2017).[2] J. Kawai, M. Takami, C. Satoko, Phys. Rev. Lett. 65, 2193–2196 (1990).[3] K. Sakurai, H. Eba, Nucl. Instr. Meth. Phys. Res. B199, 391–395 (2003).

Analysis of Th and U in thorium-based mixed-oxide fuel using wavelength dispersive X-ray fluorescence spectrometer

A precise and accurate compositional characterization methodology using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry for mixed oxide nuclear fuels is reported. The methodology involves pelletization of standards and samples. The calibration plots were made by plotting the percent intensity of analyte X-ray lines against their amount percent. The relative standard deviation were 0.4% and 0.25%, respectively for uranium and thorium, having U ranging from 2.85 to 4.2 (wt%). The analytical results were compared with chemical analysis method and were in good agreement. The developed WDXRF method is non-destructive, fast and better in comparison to chemical analysis methods.

浅谈波长色散X射线荧光光谱仪的检定

浅谈波长色散X射线荧光光谱仪的检定

A color x-ray camera for 2-6 keV using a mass produced back illuminated complementary metal oxide semiconductor sensor.

There are several reports in the scientific literature of the use of mass-produced charge coupled device or complementary metal oxide semiconductor (CMOS) sensors as x-ray detectors that combine high spatial resolution with significant energy resolution. Exploiting a relatively new especially favorable ambient-temperature back-illuminated CMOS sensor, we report the development of a spectroscopic x-ray camera having particularly impressive performance for 2-6 keV photons. This instrument has several beneficial characteristics for advanced x-ray spectroscopy studies in the laboratory, at synchrotron light sources, at x-ray free electron lasers, or when using pulsed x-ray sources such as for laser plasma physics research. These characteristics include fine position and energy resolution for individual photon events, high saturation rates, frame rates above 100 Hz, easy user maintenance for damaged sensors, and software for real-time processing. We evaluate this camera as an alternative to traditional energy-dispersive solid-state detectors, such as silicon drift detectors, and also illustrate its use in a very high resolution wavelength-dispersive x-ray fluorescence spectrometer (i.e., x-ray emission spectrometer) that has recently been reported elsewhere [W. M. Holden et al., Rev. Sci. Instrum. 88(7), 073904 (2017)].

Sulfur Chemical State and Chemical Composition of Insoluble Substance in Soft Rime, Hard Rime, and Snow Collected in Remote and Rural Areas in Japan Using Wavelength-dispersive X-ray Fluorescence.

Using a commercially available wavelength-dispersive X-ray fluorescence (WDXRF) spectrometer, the chemical composition and S-Kα spectrum of rime and snow samples collected in remote and rural areas of Japan were measured with a membrane filter sample technique to investigate the long-range transport of aerosol from the East Asian continent. Insoluble substances are derived into three categories: 1) conventional mineral origin (crustal substance), 2) urban dust origin (Fe-Zn-Ca) and 3) coal origin (S-As). Assuming that (i) S(VI) was found as a plaster-like substance in hard rime, depending on [Ca], and that (ii) S(-II) was found as non-crustal sulfur compounds, fractions of S(VI) and S(-II) in rime could be calculated as 35 ± 6 and 66 ± 7% by [Ca], which is in agreement with 32 ± 8 and 68 ± 8%, respectively, by the chemical shift of the S-Kα line. During a one-day meteorological event that included the accumulation of both rime and snow, differences to the snow-like content corresponded to characteristics typical of rime since the chemical compositions of rime also includes the composition of the snow. The fractions of 22 ± 12% of S(VI) and 76 ± 12% of S(-II), respectively, were found in rime. The fraction of S(-II) decreased from the Chugoku district towards the Shikoku district. Along the coast of the Japan Sea, the fraction of S(-II) decreased from Chugoku district toward the Northeast Japan. It can be proposed that other analytical techniques of S, Al, and Ca in that are favorable to this fractionation.