22 Analytical Instrumentation
Chemical Ionisation (HR-CI) Source Introduced for Pegasus GC-HRT
Analysis of Sulphur in Automotive Fuels by ASTM D2622-10
Rigaku Corporation (USA) recently announced the publication of a new application report describing the analysis of low concentration sulphur in automotive fuels using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry. Rigaku Application Note #XRF 5035 adheres to the American Society for Testing and Materials method ASTM D2622-10 (“Standard Test Method for Sulphur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry”) and highlights the capabilities of the Rigaku Mini-Z Sulphur analyser.
Recent developments in ultra-low sulphur diesel (ULSD) fuel have improved fuel efficiency and created cleaner emissions. The allowable limit of sulphur in fuel oils has been reduced by as much as 15 ppm in many countries, with the likelihood of further restrictions still to come.
LECO Corporation (USA) is pleased to announce a chemical ionisation (HR-CI) source for the Pegasus GC-HRT (high resolution time-of-flight mass spectrometer). This field upgradable option empowers users to dramatically change their high resolution GC/MS information with never before seen mass accuracy and resolution on pseudomolecular ions. The Pegasus GC-HRT is available with both electron ionisation (EI) and HR-CI sources, providing the option of comparison with classic NIST spectra (EI), and preservation of the molecular ion (HR-CI).
"We are excited to announce the availability of this traditional source for our Pegasus GC-HRT,” said Dr. Lorne Fell, Product Manager, LECO Separation Science. “We believe that it will take molecular ion confirmation to a whole new level when combined with the power and capabilities of the GC-HRT."
“For scientists performing petroleum analyses or metabolomics research, the addition of HR-CI makes possible identification of molecular ions and permits the robust assignment of molecular formula enhanced by the resolution and isotope ratios,” said Dr. Jeff Patrick, Director of Marketed Technologies, LECO Separation Science. “This is useful in many other fields of analysis, including environmental, dioxins, and food safety.”
Together, the CI source and the Pegasus GC-HRT provide a complete package for high-throughput/high-information content analysis, with resolution up to 50,000 FWHM, mass accuracies less than 1 ppm, and acquisition rates up to 200 spectra/second—all with high-integrity isotopic abundance measurements to facilitate rich information content and high-confidence analyte identification. ChromaTOF-HRT software utilises True Signal Deconvolution for accurate peak identification, seamless data handling, and compatibility with the NIST library.
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For compliance verification, X-ray fluorescence (XRF) spectrometry is the preferred analysis tool for use at distribution terminals, as well as at mobile or stationary testing laboratories. Application Note #XRF 5035 details sample preparation, method calibration and repeatability. For the analysis described in the report, 4 ml of each sample was poured into a special
liquid cell with a 2.5 µm Mylar analysis film. “Number 2 diesel fuel” standards and isooctane-based standards were used for calibration for diesel fuel and gasoline respectively.
Measurements were carried out using the Mini-Z Sulphur analyser, a benchtop single fixed-channel WDXRF spectrometer designed to minimise installation requirements such as cooling water, power supply and floor space. It has a built-in control panel designed for easy operation. The Mini-Z Sulphur analyser is equipped with an air-cooled 40 W Cr-target X-ray tube. The RX-9 analysing crystal is optimised for sulphur analysis.
The results show that low concentration sulphur in petroleum-based fuel can be routinely analysed with high precision using the Mini-Z Sulphur analyser, meeting the requirement of the current ASTM D2622-10 method.
A copy of this application report may be requested on Rigaku’s official website at:
http://j.mp/ZGIyz7 Reader Reply Card No 71
Worldwide Trusted Source for Calibration Standards
Analytical Services (USA) is a worldwide trusted source for calibration standards serving the petroleum, lube oil, crude oil and polymers industry since 1993. Their Quality Management System is now certified to ISO 9001. You can visit their website for a downloadable catalogue and to send any custom requests.
Although Analytical Services (AS) have many standards and calibration sets available as catalogue items, they can also provide custom sets based on your specific needs. AS specialise in the custom formulation of multi-element standards in difficult matrices. A complete line of consumables such as film, cups and pipets necessary for XRF analysis, is also offered. Their manufacturing facility is located just north of Houston, and they ship worldwide into almost every country. AS are fully certified in the shipment of dangerous goods and their customer service staff is prepared to assist with ordering, technical assistance and any questions you may have regarding their products and services. All standards are produced and certified in-house and are accompanied with a Certificate of Analysis indicating traceability to ASTM and NIST methods, validity term and degree of uncertainty.
Reader Reply Card No 73 New Age in Flashpoint Testing
MINIFLASH TOUCH is the latest addition to the AMETEK Grabner Instruments (Austria) line of portable flashpoint testers that combines all of the field-proven advantages of the MINIFLASH tester line with a new full colour touch screen design. The MINIFLASH series is a uniquely designed group of flash-point testers that uses a continuously closed cup method to determine the flash point of petroleum products, liquids and solids.
The MINIFLASH method offers the highest repeatability and reproducibility, an excellent and ASTM-proven correlation*) to the D93 Pensky-Martens method. It delivers results equivalent to other well-known, closed-cup standards. Typical applications include the fast screening of diesel and jet fuels; the flash-point testing of potentially flammable goods, pharmaceuticals, aroma products, paints, varnishes, engine and lubricating oils; and the determination of solid waste composition and unknown mixtures of liquid hydrocarbons. The unit’s compact size and rugged housing make it the perfect solution for military applications, mobile labs and other demanding applications.
The MINIFLASH TOUCH utilises Ignition Protection Technology for maximum safety during flashpoint tests. This Grabner- developed method measures the instantaneous pressure increase inside a continuously closed test chamber resulting from an electric arc that ignites vapour from a 1 or 2 mL sample. No open flame is produced. Automatic explosion probing and automatic interruption of oxygen supply after flashpoint detection make the MINIFLASH the safest flashpoint tester available. The instrument’s innovative design also eliminates offensive fumes in the testing area and reduces sample waste.
For a quick sample turnaround and extended instrument life, Grabner Instruments developed Peltier Protection Technology, an advanced and fast thermoelectric heating and cooling regulation technology that extends the measuring temperature to well above 400°C and optimises performance and lifetime of the Peltier cooling.
Grabner Instruments has also developed Combustion Analysis to visualise the presence of contaminants and small concentrations of flammable compounds in samples. This gives users the opportunity to follow every millisecond of the flash combustion in unprecedented detail and makes the MINIFLASH suitable for flash-point testing of contaminated samples, biodiesel fuels and other difficult applications.
*) ASTM Statement on the Grabner Instruments ASTM D7094 standard versus ASTM D93A: “There is no statistically significant bias observed between ASTM D7094 and ASTM D93 Procedure A.”
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APRIL / MAY 2013 •
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