22 Analytical Instrumentation
Analysis of Low Concentration Sulphur in Petroleum-Based Fuels by Benchtop WDXRF
Rigaku Corporation (USA) is pleased to publish a new application report highlighting the performance of the Rigaku Supermini 200, the world’s only benchtop wavelength- dispersive X-ray fluorescence (WDXRF) spectrometer and the latest in a series of revolutionary compact WDXRF systems from Rigaku. Application Note #5044 details the analysis of petroleum-based fuels for low concentrations of sulphur by benchtop WDXRF. The new method complies with ASTM D2622 – 10: Standard Test Method for Sulphur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry.
Sulphur in petroleum-based fuels contributes to atmospheric pollution. Sulphur content in fuels is strictly controlled and regulation of sulphur content in fuels, including diesel fuel
and gasoline, has been tightened. The accurate measurement of sulphur content in fuel oil is, therefore critical, for refineries. X-ray fluorescence (XRF) spectrometry is used for quantitative analysis of sulphur in petroleum-based fuels, due to its simple sample preparation requirements.
The new application note covers sample preparation, method calibration and repeatability, and demonstrates that low concentration sulphur in petroleum-based fuel can be routinely analysed with excellent accuracy, sensitivity and repeatability using a benchtop WDXRF spectrometer with minimal site requirements.
For this application, four millilitres of each sample was poured into a standard liquid cell. “Number 2 diesel fuel” standards were used for calibration of diesel fuel, gasoline and kerosene. Two aliquot quantities of the sample were prepared and quantified with the calibration. The process was repeated twenty times.
The Rigaku Supermini200 benchtop WDXRF system, which can be plugged into a standard wall receptacle and does not require cooling of the X-ray tube or the power supply, is shown to meet specifications of the test method.
A copy of this application report may be requested on the official Rigaku website at
http://j.mp/XAxpTz. Reader Reply Card No 79
Automatic Flash Point Tester with Integrated Fire Extinguisher
Petrotest (Germany), a company of Anton Paar, now offers the PMA 5 Pensky-Martens (ASTM D93) flash point tester that performs flash point testing of petroleum products using Pensky-Martens closed-cup ASTM D93 A, B and C methods. PMA 5 can be used for both biodiesel and biodiesel blended fuels along with such distillate fuels as diesel, heating oil and kerosene and such potentially flammable liquids as lubricating oils, paints and varnishes.
With an integrated fire extinguisher as a standard delivery item, PMA 5 highly improves user safety. Among the features of this highly versatile bench-top instrument are an over-temperature protection circuit, splash-
proof membrane key panel, and a built-in sensor for automatic barometric pressure correction. The PMA 5 also offers both gas and electric ignition options as standard. In addition, the instrument features a convenient to use multi-function head for easy, one-hand, simultaneous connection of all sensors and actuators.
Among the advantages of the PMA 5 is its ability to heat samples, while the instrument performs tests unattended. Heating keeps samples with a high-melting point at temperatures above 150o testing begins. This saves time and makes cleaning easier.
C, allowing for the immediate start of the stirrer when flash point
PMA 5 comes completely ready for testing with automatic test routines, user definable programs as well as a rapid search program. The easy-to-operate analyser features the latest electronics, including a 5.7-inch colour graphics display and Pmove jog wheel for input of e.g. test parameters, sample name and program selection.
It has selectable output, either °C or °F, and a measuring temperature testing range from ambient to 405°C (761°F) without requiring any additional equipment.
Reader Reply Card No 80
The amount of benzene in gasoline is a concern because it is a known human carcinogen, and exposure to it has been linked to detrimental health effects. The challenge with the analysis lies in the complex composition of gasoline, which consists of hundreds of different compounds. Reformulated gasoline also contains additives to produce more complete combustion and subsequent lower emissions of harmful compounds. These additives accomplish this by boosting the oxygen content, and are commonly referred to as "oxygenates". Ethanol is a commonly used oxygenate. Therefore, to measure benzene in reformulated gasoline, it must be resolved from the C5-C12 aliphatic portion, other aromatics, ethanol and any method required internal standards. This typically requires the use of a two-column switching procedure.
Analysis of a reformulated gasoline sample, from Supelco (USA), on the extremely polar SLB-IL111 capillary column resulted in the elution of benzene after the aliphatic portion, and also resolution of benzene and ethanol. Additionally, the phase stability of the SLB-IL111 column exhibits a stable baseline when subjected to a temperature ramp. Because this column can be used up to 270 °C, it also allows the timely elution of the heavy aromatic constituents in gasoline. These observations indicate that the SLB-IL111 may be an effective alternative to the two-column switching procedure currently required for the determination of benzene and other aromatics in reformulated gasoline.
Reader Reply Card No 81
A Single-Column Application for the GC Determination of Benzene
Reader Reply Card No 82 Annual Buyers’ Guide 2013 •
www.petro-online.com
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