POWER + FLEXIBILITY IN ELEMENTAL ANALYSIS

Transcription

1 POWER + FLEXIBILITY IN ELEMENTAL ANALYSIS

2 Energy Dispersive X-Ray Fluorescence Spectrometry (EDXRF) is an atomic spectroscopy that provides elemental composition analysis of materials. The elemental range of EDXRF is from Sodium (Na) through Uranium (U). Virtually any sample can be analyzed for elemental composition with EDXRF solids, liquids, powders, and slurries. ANALYSIS PROCESS. X-rays from an X-ray tube source are shined on the sample. The atoms that make up the sample are excited and emit X-rays, they fluoresce. If the sample is thick, composition is measured. If the sample is thin, thickness and composition are measured. The analysis is non-destructive, X-rays do not change the sample. WITHIN THE ATOM. Inner Shell electrons are ejected by incident X-ray photons (excitation). Outer shell electrons replace the inner shell electrons of the excited atom. These electron transitions result in the emission of X-ray photons, the energies of which (E), are characteristic of the emitting atom s atomic number (Z). These X-rays are detected and the elements are identified (Eα Z). The frequencies of these emissions, peak intensities, tell us how much of each element is present, concentration. THE TECHNOLOGY X-RAY FLUORESCENCE SPECTROMETRY 100 Effect of Thickness on Intensity Relative Intensity Infinite Thickness Thickness (µm) BEAM FILTERS. Beam filters remove background, thereby, enhancing analyte sensitivity. Detection limits are a function of peak-to-background response. SAMPLE THICKNESS. Peak intensity increases logarithmically to sample thickness. When the sample is infinitely thick, the intensity is constant. Sample thickness can be measured when the sample is less than infinitely thick. DETECTOR. High resolution solid-state lithiumdrifted Silicon [Si(Li)] detector sees all X-ray events providing simultaneous multielement analysis. KevexSpectrace is an operating division of NORAN Instruments Inc. KevexSpectrace represents 5 decades of Energy Dispersive X-Ray Fluorescence (EDXRF) development, manufacturing, applications expertise and customer support with strategically located facilities worldwide. The name, KevexSpectrace is synonymous with high performance, highly reliable EDXRF products count on us.

3 APPLICATIONS FROM DIRT TO HIGH TECH DEVICES SOIL. Analysis and remediation of hazardous waste sites requires determination of the nature, extent and magnitude of the contamination. QuanX provides rapid identification and analysis of priority metal contaminants that are present in the soil. Our low maintenance system with no-ln detector is easily transported to the field for on-site determinations, thus quickly defining the amount of sampling required and saving days and sometimes weeks in analytical turnaround time. As a result of the technique being non-destructive, analyzed samples can be retained for further analysis. INDUSTRY. Petroleum cracking catalysts are contaminated by transition metals in the oil feed stocks. QuanX provides routine monitoring of metal content in the feeds allowing refiners to optimize the life of their catalysts. Aerospace, automotive and heavy equipment manufacturers must verify that incoming components are of the specified alloy. The intensity matching capabilities of QuanX make alloy verification fast and easy. HIGH-TECH. QuanX provides semiconductor manufacturers and data storage device manufacturers a rapid and precise means of controlling thin-film deposition processes. Our thin-film measurement algorithms provide non-destructive thickness and composition metrology of single-layer or multi-layer stacks. Sample handling options automate multiple device or multiple point analysis. OTHER APPLICATIONS INCLUDE Air aerosol particles on filter membranes Hazardous waste and sludge Wear metals in lubricants Refined precious metals Plating bath composition Metal plating thickness and composition Catalyst residue and additives in polymers Geological ores, ore processing and mineral composition Conservation and archeology If your application is not listed on this page call us! (650)

4 QUANX FEATURES FLEXIBILITY An important feature of X-ray spectrometry is that it is non-destructive. To fully exploit this feature, QuanX has a sample chamber that is large enough to accept the specimen without alteration, reliably position the sample to the analysis plane, move a sample to various positions keeping the analysis plane in focus should multiple analysis points be required, or reliably position multiple samples to the analysis position on the analysis plane. QuanX features a large sample chamber with numerous sample handling options.

5 UNIQUE CORE TECHNOLOGY PELTIER-COOLED SI(LI) X-RAY DETECTOR We introduced the EDXRF community to the Electrically-Cooled Detector (ECD). This innovation still has no match in performance and convenience. No Liquid Nitrogen Low maintenance Compatible with most environments in the laboratory, near process, clean room, or transported to the field. No sacrifice in performance QUANX BENEFITS The standard chamber is 30.5cm Wide x 38.9cm Deep x 6.6cm High and will accept micro samples to massive samples that will fit within these dimensions. Optionally, extended-height lids are available for tall samples. For multiple sample handling, QuanX is configured with a 20-position tray. Each position is 31 mm in diameter (an XRF standard) to accept pressed pellets, or polymer cups for liquid or loose powder samples. For multiple sample handling of larger samples, QuanX is configured with a 10-position tray that accepts our sample spinner platform, which is configurable for samples up to 47 mm in diameter and can spin the sample during analysis to homogenize the excited volume. Meeting Specific Analytical Needs: Multiple hard disk analyses are handled with 4 and 8-position disk holders. Film thickness and composition measurements are made quickly and automatically on many samples. When many points on a single disk need to be measured, QuanX is equipped with a programmable r-theta stage. If the substrate media is a Silicon wafer, our y-theta stage replaces the r-theta stage for film thickness/composition uniformity evaluations. The eight position thin-film standards tray accommodates specially mounted reference materials. Trace elemental analysis (ppb levels) of aqueous samples or trace surface contamination on silicon wafers, are measured using the Microsample X-ray Analysis (MXA) technique. Residues from micro aliquots of water or Vapor Phase Decomposition (VPD) etch from silicon wafer surfaces are automatically measured (18 samples) with the QuanX MXA x-y stage.

6 Wintrace XRF application software is designed to provide the analyst an optimum combination of flexibility and ease of use for setting up analysis procedures and obtaining accurate results whether it be for routine process control samples, complete unknowns, or new materials in an R&D environment. Wintrace is a complete XRF package featuring: Standardless Analysis Semi-Standardless Analysis Fundamental Parameters (FP) and empirical methods with standards Multi-layer thickness and composition No limit on the number of elements No limit on the number of standards Multiple excitation conditions with automated operation Wintrace is easy to learn and even easier to operate! WINTRACE RESULTS DRIVEN SOFTWARE THE WINTRACE SUITE. Define analysis methods, evaluate standards data, and customize analysis reports with Method Explorer. Once the method is complete, Acquisition Manager is used to obtain results periodically or continuously. Multiple methods can be stored for varying sample types. The System Configuration program defines the specific hardware of your system. Analytical reference material data are entered only once and maintained with the Standards Library program. Method Explorer guides you through the analysis setup process to achieve optimum instrument settings and data processing. Method categories are displayed in the method bar on the left of the screen for easy access. The calibration category displays the standards table, which lists the standards and elements selected for the analysis. A red color code flags elements for which a set-up problem exists. This is part of the Wintrace Method Integrity Protection design simple and error free. Results are quick and easy with Acquisition Manager. The operator simply sets up the analysis tray with sample identification, predefined analysis method and tray position, and then starts the acquisitions. Even different types of samples can be run in the same tray with our mixed grill operation, a powerful innovation.

7 NEVER COMPROMISE PERFORMANCE Pb by EDXRF (PPM) Accuracy Sulfur concentration (ppm) Precision of Sulfur Analysis 325 ppm sample measured over six days n=826 avg=323 (ppm) stdev=12 (ppm) rsd=3.7% LLD (ppm) Lower Limits of Detection Matrix Hydrocarbon Aqueous Geologic Pb by ICP (PPM) Replicate Analysis (300 sec Livetime) Atomic Number ACCURACY. Many variables affect the accuracy of an instrumental analysis. The QuanX system with Wintrace provides proven algorithms for accurate processing of spectra and quantification. Always a factor in EDXRF, as with other instrumental methods, is the quality of the standards that are used. The wide dynamic range and the penetrating characteristics of X-rays minimize and in some cases eliminate the need for sample preparation in EDXRF analysis. Errors introduced by sample digestion and dilution often associated with other methods are eliminated. The EDXRF data for the correlation graph presented above were acquired from soil samples prepared simply by grinding and analyzing as loose powders. PRECISION. System stability is the basis for precise results. With the superb stability of QuanX (short term and long term) analytical precision becomes a set-up parameter. Unlike other spectroscopic techniques, the precision of a QuanX EDXRF measurement can be optimized to meet the requirement of the application. Improved precision is attained by optimizing countrate, reducing background and adjusting analysis time parameters that are easily accessed with Wintrace Method Explorer. Data for the example presented above were continuously acquired over a period of six days. SENSITIVITY. EDXRF sensitivity is influenced by both system performance and the sample composition (sample matrix). QuanX provides the analyst with high resolution solid-state detection and excitation control to optimize analyte peak-to-background response. Matrix effects are primarily the result of absorption of the analyte emission by the sample matrix. Sample matrices of higher average atomic number are more absorptive and reduce analyte sensitivity as shown in the figure above. For instance, the sensitivity expressed as lower limit of detection for a metal such as nickel in oil is much better than for nickel in steel. Detection limits for metals in oil are as low as 0.5 ppm. In heavier matrices, such as soil, detection limits for typical analysis times are less than 5 ppm. Part per billion sensitivities can be achieved for aqueous samples using the Microsample X-Ray Analysis (MXA) techniques.

8 QUANX SYSTEM SPECIFICATIONS Sample Chamber Sample Types Dimensions Single Sample Tray 20-Position Sample Tray (optional) 10-Position Sample Tray with Spinner (optional) Environments Excitation Solids, powders, liquids, filtrates, thin films, and others cm (12.0") wide X 38.9 cm (15.3") deep X 6.6 cm (2.6") high, extended chamber (optional): 21.5 cm (8.6") or 37.1 cm (14.6") high. Samples to chamber size with latitude for multi-point analyses. Samples to 31 mm diameter. Samples to 47 mm diameter. Automated and manual sample trays for special samples such as semiconductor wafers and computer disk media are available. Air, vacuum (optional), and helium (optional). Vacuum is required for analysis of lower concentrations of elements with atomic numbers less than 22. Helium is required for these elements in liquids (3.5) (11.0) 2.79 (1.1) (28.3) (16.2) X-ray Tube X-ray Generator System Stability Filters Beam Collimators (optional) Detection Rh target, 125 micron Be window, air cooled. Other targets available kv in 1 kv increments. Current adjustable in 0.02 ma increments to 2.0mA from 4-25kV to 50W from 26-50kV. 0.25% over any 8 hour period. Automated selection of 7 filters plus an open position. 1mm, 3.5 mm and 6.8 mm. For analysis of small areas or samples (28.85) (20.4) Chamber Lid Lift Lid Thermoelectric Cooled (optional) Liquid Nitrogen Cooled Window Thickness Solid state, Si(Li), 15mm2 area, 170 ev resolution for 5.9 KeV x-rays. Solid state, Si(Li), 30mm2 area, 155 ev resolution for 5.9 KeV x-rays, 8 liter dewar. Thermoelectric cooling: 12 microns; LN cooling: 8 microns (33.1) Data Acquisition Pulse Processor Analog to Digital Converter Data Memory Data Processor Time variant shaping network, computer selected count rate range. 4,096 addresses, 100 mhz clock, automated calibration. 2,048 data addresses, 16 million counts/channel. Current PC technology, and Color Graphics Printer. Software Display Output Automation Spectrum Processing Analysis Techniques Operating System X-ray spectrum, overlapped spectra comparison, peak identification markers, peak labels, and analysis parameters. CRT, graphics printer, and modem. Chamber environment, x-ray source output, filter selection, multiple excitation conditions and sample selection. Automatic element identification, digital filter background removal, least squares empirical peak deconvolution, gross peak intensities, and net peak intensities above background. Empirical and fundamental parameters methods. Normalization to a check standard and display plots of calibration curves are included. Microsoft Windows 98, Windows NT 4.0 or later compatible (21.5) 4.57 (1.8) Dimensions/Weight Height cm (16.2"). Width cm (28.3"). Depth cm (23.3"). Weight 90.7 kg (200 lbs.). Note Does not include PC or vacuum option. Utility Requirement Power Telephone 100, 115 or 230 VAC, 50 or 60 Hz, 1000 watts watts with vacuum option. Data quality line required for modem diagnostics and remote monitoring. Environmental Temperature Humidity 0 to 32 C (32-90 F) % RH (non-condensing). 855 Veterans Blvd, Redwood City, CA or Phone Fax W. Beltline Highway, Middleton, WI Phone Fax International customers contact KevexSpectrace for local distribution KevexSpectrace, Inc. 07/00 All trademarks are the property of their respective companies.