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22 XRF Feature Figure 6. ASTM Interlab Crosscheck Data for Reformulated Gasoline 2015


Note that the precision statements for ASTM D7039 for the MWDXRF technique are based on the range of the method, 3.2 to 2822 ppm, which far exceeds the needs, when interested in measuring sulfur in finished product such as highway diesel or gasoline. If the results of Interlaboratory Study #761, gathered and analyzed in accordance with ASTM D6300 methodology for sulfur samples limited to ≤25 ppm S, it can be shown that the Repeatability (r) = 1.1 ppm and the Reproducibility (R) = 1.3 ppm.


Conclusions


When considering technologies for process analyzers, the most important characteristics of a good analyzer are reliable performance, a high degree of up time, superior stability, and good reproducibility, especially in the range of ≤10 ppm for sulfur. Having the lowest possible detection limit is not as valuable as having good precision at the control target. When used for


process control, small biases can be accounted for, as long as the process analyzer operates consistently within the control limits. An analyzer with simple construction, ease of maintenance, and ability to correlate closely with lab methods should be important in the selection process. Also important to remember is that no process analyzer is subject to “laboratory conditions” so the performance of the lab instrument may not be a good indicator of how the process version will perform in the field. A sulfur monitoring solution that minimizes or eliminates moving parts, gas cylinders, and scheduled maintenance and calibration events is ideal for process analyzers that cannot be maintained as frequently as lab equipment. When regulations limit the maximum sulfur concentration, a preferred technique is one that produces repeatable and reproducible results, while reducing the frequency an analyzer needs to be cross checked with laboratory measurements and allows refiners the confidence and flexibility to change process variables knowing that they have a precise measurement of the sulfur content in their process streams. While the EPA has sanctioned WDXRF as the primary testing technology, there is no process analyzer that measures strictly with this technique. However, process analyzers utilizing MWDXRF, a subset of WDXRF, are available and have been in service in the field since 2005. These analyzers were initially used for process control of sulfur in ULSD highway diesel but have since been used on naphtha streams and in gasoline blending. These analyzers have proven to be very reliable, simple to maintain, and correlate very closely with laboratory methods. The method does not require gaseous consumables so the cost of ownership is low. MWDXRF is the only WDXRF solution available for process. Validated in reproducibility tests, it is ready and proven for applications below 10ppm and even further (5ppm).


For additional information about how XOS can help with Tier 3 compliance, please visit our website at www.xos.com or contact us at info@xos.com.


This paper was originally presented at the 2016 ISA Analysis Division Symposium.


Author Contact Details Shaun Spiro, XOS • 15 Tech Valley Drive, East Greenbush, NY 12061 USA • Tel: 518-880-1500 • Email: sspiro@xos.com • Web: https://xos.com


Intelligent and Standardless Software for Wide Ranging Elemental Analysis


With modern XRF analysis there are two major analytical strategies: conventional calibration and standardless analysis. When working with known sample materials and when highest precision and accuracy are in demand, a standard-based calibration delivers best results. However, almost all labs are faced with unknown samples now and then or with samples for which no reference material is available. In these situations standardless analysis provides an effective tool to analyse elemental composition. This is only possible with powerful standardless software. Bruker AXS’ (Germany) new SMART-QUANT FP is offered as a fully integrated component of the S2 PUMA’s Spectra Elements instrument software package and delivers reliable elemental data from C to U for solid, fused, pressed, powdery or liquid material without the need for laborious calibration.


SMART-QUANT FP uses fundamental parameters to calculate theoretical spectra based on given sample and instrument parameters and detector response. The software then compares the theoretical with the measured spectrum and minimises differences between them by adjusting the element concentrations in its model. This iterative process is continued until a perfect match between the theoretical and the measured spectrum is found. All this is carried out fully automated in the background so that the operator does not have to worry about it. However, if one wishes to do so, the process can be constrained by the input of a variety of parameters to tune the standardless calibration to the application’s needs.


To start a measurement in its simplest form, place your sample into the spectrometer, enter a sample name and press ‘Start’. That’s it. After a few minutes you will have your results. For specific user and application needs measurement parameters can be adjusted to fit the respective analysis requirements. The software allows a wide range of customisations with regards to sample definition, measurement specifications, analysis scheduling, and result presentation. To further tailor the hardware towards your specific applications needs, the S2 PUMA can be ordered with different X-ray tubes, several detector options, and variety of sample handling options.


ADVANCED SULFUR ANALYSIS


The best in sulfur analysis on the bench or online.


From ultra-low sulfur measurement in gasoline and diesel fuels to high-pressure process and pipeline sulfur analysis, AMETEK has the solution for you. Our ASOMA Phoenix II XRF analyzer offers a detection range down to 1.5 ppm sulfur, which covers both current and proposed federal EPA limits for sulfur in gasoline. And our ASOMA 682T-HP


online sulfur analyzer eliminates the need for sample handling while providing low cost of ownership. It’s ideal for crude and other highly viscous hydrocarbons in pipelines, terminals, and blending operations.


For More Info, email: email:


For More Info, email:


For the best in benchtop and online sulfur analyzers, visit ametekpi.com today. © 2016 AMETEK Inc. All rights reserved.


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682T-HP XRT Online Sulfur Analyzer


Phoenix II XRF Analyzer for Elemental Analysis


Nevertheless, SMART-QUANT FP is set up in a ‘one fits all’ standard configuration to let you start measurements immediately without lengthy adjustments. The intuitive user interface guides the operator through the process from placing the sample through result handling, be it an out-of-thebox standardless application or a more advanced analysis program. Essential results are displayed immediately after the measurement in the ‘Loader’ tab. More detailed analytical information is provided in the ‘Results Manager’ (see Figure 2). Every sample is displayed in a dedicated window where all analytical data can be viewed without scrolling. This includes detailed analytical information and measured as well as fitted spectra. The goodness of the fit can be judged on a displayed figure of merit ‘R/R0’.


This system offers quick, accurate and precise analysis of unknown samples without calibration. Users will appreciate its analytical flexibility, whether they are analysing solid, fused, pressed, powdery or liquid samples, SMARTQUANT FP can handle all of them. This instrument’s operator-friendly user interface guarantees a fast and straightforward measurement setup and an integrated results viewer offers quick and easy data access. Advanced analysis settings allow for customised measurement and preparation conditions to further increase analytical performance. SMARTQUANT FP performs a seamless integrated solution within the spectrometer software with no lengthy installation required.


For More Info, email: email:


For More Info, email: email:


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