A non-invasive method of X-ray fluorescence (XRF) spectrometry was employed to analyse the alloy composition of 38 explanted generators made by 9 different manufacturers: 21 generators for PMs (20 models from 6 manufacturers) and 17 generators for ICDs (17 models from 6 manufacturers). A non-metallic abrasive paste was used to remove the superficial ‘corrosion’ layer from the analysed part of each device. The analysis was performed with a manual XRF spectrometer Delta Professional manufactured by the Olympus Corporation (Waltham, Massachusetts, USA), which was placed into a Flex Stand in the ‘Analytical Plus’ settings. The X-ray tube had the following characteristics: the voltage up to 40 kV, the power of 4 W, and the exciting current of 200 μA. The silicon drift detector (SDD) was primarily calibrated on the surface of 3 mm2, allowing both qualitative and quantitative analysis of the following elements: aluminium, antimony, bismuth, chromium, cobalt, copper, gold, iron, lead, magnesium, manganese, nickel, niobium, phosphorus, silicon, silver, sulphur, tin, titanium, vanadium, zinc, and zirconium. Each sample was measured three times, and mean values were calculated from the measured values. Metal concentrations in the alloys were expressed in percentage (%). The aim of the analysis was to select metals to be tested for hypersensitivity reactions.
Delta professional
Manufactured by Olympus
Sourced in Japan
The Delta Professional is a versatile and precision laboratory equipment designed for a wide range of scientific applications. It features advanced technology and engineering to provide accurate and reliable performance. The core function of the Delta Professional is to enable precise measurements, analysis, and data collection in laboratory settings.
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6 protocols using delta professional
1
XRF Analysis of Explanted Generator Alloys
2
Comprehensive Characterization of Silica Cake
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Sampling was conducted throughout every stage of the process and
during repeated operations to ensure both process efficiency and consistency.
Analysis was conducted off-site. Solution concentrations of contaminants
were determined by inductively coupled plasma optical emission spectrometry
(ICP-OES) (Analytikjena PQ9000 Elite, [U]LOD = 5 μg
L–1) in a 5% nitric acid media. Bulk mineral phases
and solid contents were determined by X-ray powder diffraction (XRD)
(Bruker, D2 Phaser) and X-ray fluorescence (XRF) (Olympus, Delta professional),
respectively. The moisture content was determined by thermogravimetric
analysis (TGA) (TA Instruments Korea, SDT Q600) up to 150 °C
at a ramp rate of 10 °C min–1. Radioactivity
of the final silica cake was determined by an α-spectrometer
(Alpha Analyst, CANBERRA). Scanning electron microscopy coupled with
energy-dispersive X-ray spectroscopy (SEM/EDS, Bruker Nano, Xflash
Detector 410-M) was used for morphological and elemental analysis
of particulate samples. Solution nephelometric turbidity units (NTU)
was measured using a Hanna HI 98703 turbidity meter as an indication
of solution clarity.
during repeated operations to ensure both process efficiency and consistency.
Analysis was conducted off-site. Solution concentrations of contaminants
were determined by inductively coupled plasma optical emission spectrometry
(ICP-OES) (Analytikjena PQ9000 Elite, [U]LOD = 5 μg
L–1) in a 5% nitric acid media. Bulk mineral phases
and solid contents were determined by X-ray powder diffraction (XRD)
(Bruker, D2 Phaser) and X-ray fluorescence (XRF) (Olympus, Delta professional),
respectively. The moisture content was determined by thermogravimetric
analysis (TGA) (TA Instruments Korea, SDT Q600) up to 150 °C
at a ramp rate of 10 °C min–1. Radioactivity
of the final silica cake was determined by an α-spectrometer
(Alpha Analyst, CANBERRA). Scanning electron microscopy coupled with
energy-dispersive X-ray spectroscopy (SEM/EDS, Bruker Nano, Xflash
Detector 410-M) was used for morphological and elemental analysis
of particulate samples. Solution nephelometric turbidity units (NTU)
was measured using a Hanna HI 98703 turbidity meter as an indication
of solution clarity.
3
Elemental Composition of Bat Guano
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The elemental compositions of bat guano C1 and C2 were analyzed semi-quantitatively using handheld X-Ray Fluorescence Spectrometer (Delta Professional, Olympus, Japan) at the Earth Material Science Laboratory of the National Institute of Geological Science, University of the Philippines Diliman. Guano samples were dried at 105°C and elemental analysis was done in triplicates. Light elements, Silver (Ag), Cadmium (Cd), Tin (Sn) and Antimony (Sb) were removed to normalize the results and reported as semi-quantitative or based on a relative composition.
4
Comprehensive Material Characterization Protocol
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Chemical composition analysis and observation of metallographic structures were performed using plate specimens prepared in the same manner as the preparation of the specimens for the immersion tests. Chemical composition analysis was performed by fluorescent X-ray analysis (XRF) and X-ray diffraction (XRD). XRF was performed with a fluorescent X-ray analyzer (DELTA Professional, OLYMPUS, Tokyo, Japan). XRD was performed using a desktop X-ray diffractometer (MiniFlex, Rigaku, Tokyo, Japan). Surface structure was observed using a digital microscope (VHX-2000, KEYENCE, Osaka, Japan). The observation was performed on three patterns: as sintered, after polishing, and after etching (acidic solution (nitric acid:hydrofluoric acid:water = 4 1:5) was used for etching).
5
Scanning Electron Microscopy and X-Ray Analysis
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The surface morphology of the electrode was examined using a JEOL JSM-6610LV scanning electron microscope (SEM) at 20 kV. Energy dispersive X-ray spectroscopy (EDS) was used to qualitatively study the chemical composition of the alloy. Elemental quantification was performed by X-ray fluorescence spectroscopy (XRF) using an Olympus Delta Professional portable XRF analyser.
6
Microstructural Characterization of Sintered Specimens
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Chemical composition analyses were performed via X-ray diffraction (XRD), with Cu Kα radiation at 30 kV and 15 mA, and X-ray fluorescence (XRF) analysis. XRD analysis was performed on the sintered specimens along each building direction using a desktop X-ray diffractometer (MiniFlex, Rigaku, Tokyo, Japan) (n = 6). XRF was performed using a fluorescent X-ray analyzer (DELTA Professional, OLYMPUS, Tokyo, Japan). The microstructures were observed via scanning electron microscopy (SEM) (JSM-IT200, JEOL, Tokyo, Japan) at an accelerating voltage of 15.0 kV, after sputter-coating the specimens with platinum under an argon gas environment using a sputter-coater machine (E-1030, Hitachi, Tokyo, Japan).
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