24 Analytical Instrumentation - Focus on Sulphur Analysis
chlorine on typical EDXRF systems. This is due to the fact that as sulphur levels increase the kb emission line for sulphur will interfere with the chlorine emission, resulting in higher chlorine numbers. The data shows that above 2000 ppm sulphur, the integrated area for chlorine will start to include the shouldering peak from the high sulphur. A spectral representation of this interference is depicted in figure 4.
Figure 4: Sulphur and Chlorine Spectra Sample ID
0 Cl 0S 50Cl 0S
50Cl 0.005%S 50Cl 0.099%S 50Cl 0.21%S 50Cl 0.50%S 50Cl 1.00%S 50Cl 1.43%S
Curve A No S Correction
Cl, ppm 0.0
50.7 49.7 49.0 49.9 55.0 62.1 62.5
S, wt% NA NA NA NA NA NA NA NA
Cl, ppm 0.0
50.0 49.9 48.2 49.3 49.8 49.5 49.8
Curve B S Correction
S, wt% *0.0 *0.0
*0.004 0.098 0.21 0.49 1.01 1.43
Table 4: Analytical results for Sulphur and Chlorine (* Sulphur values reported outside the calibration range) to simultaneously measure sulphur and chlorine accurately.
The following data depicted in table 5 below are typical gas oil samples analysed on the MESA-6000.
Sample ID Gas Oil #1 Gas Oil #2 Gas Oil #3 Gas Oil #4
The samples were analysed on two calibration curves. Curve A was a chlorine only calibration curve, 0-100ppm chlorine in mineral oil. Curve B was a chlorine (0-100ppm) and sulphur (0.1 – 2wt%) calibration curve in mineral oil. Curve A displays chlorine data and the effects from sulphur interference, Curve B demonstrates how the results for chlorine were automatically corrected by software for the increasing sulphur concentrations. The results are displayed in Table 4.
The MESA-6000 clearly demonstrates its ability to not only correct for the presence of sulphur, but Conclusion
Innovative diffractive optics coupled with the simplicity of EDXRF technology define the MESA-6000 as an extremely simple instrument to operate for multiple element analysis in a wide variety of samples. The instrument’s versatility and flexibility make the MESA-6000 the instrument of choice in the petroleum and fuel industry.
Cl, ppm 4.6 4.1 3.8
10.4 Table 5: Analytical results for Sulphur and Chlorine in Gas Oil
S, wt% 3.10 2.97 3.2 1.2
Cost-effective, Rapid and Simple Analytical Solution for Sulphur in Petroleum Products
The Energy Dispersive XRF (EDXRF) Lab-X3500 from Oxford Instruments (UK) is a compact bench-top analyser that can be used in the lab, field, mobile laboratory; in fact where ever you need on site analysis operated by production staff and with full conformance to ASTM D4294.
The EDXRF X-Supreme8000 offers multi-sample analysis for “ultra low sulphur” (<10ppm) up to 5% covering all sample matrix types. In addition, the X-Supreme8000 has the flexibility to measure additional elements such as Nickel and Vanadium in fuel oil. These instruments are world renowned for simple installation, long term reliability and ease of use. This is achieved through close attention to detail on high quality design and manufacture Both the X-Supreme and Lab-X can be located anywhere, wherever confirmation of sulphur concentration is required for regulatory purposes. With X-ray tubes optimised for sulphur determination and running at minimal power all help ensure long service life, typically over ten years, leading to extremely low running costs.
Dedicated application packages cover different analytical requirements. For Ultra Low Sulphur determination (< 10mg/kg) the various ISO/ASTM test methods recommend the measurement of two aliquots (portions) of sample when measuring sulphur concentrations below 100mg/kg. On the X-Supreme8000 the software “requests” two aliquots are placed on the sample carousel, measurements are sequentially taken and the average and individual sulphur concentration results are displayed. Background “SmartCheck” software routines automatically check a number of customer defined parameters, for example; the difference in sulphur concentration between aliquots; and should the results be outside tolerance, a warning message is displayed. This all leads to high quality analysis, often with the analysis carried out by production staff. In addition to Sulphur, other elements can be measured with equal ease, for example; chlorine in platforming catalyst, lead in gasoline etc., providing a cost-effective, dependable and flexible analytical solution. For those customers requiring sulphur analysis to ASTM D2622 Wavelength Dispersive XRF (WDXRF) the MDX1000 offers simultaneous elemental analysis. Superb reliability is achieved through employing two fixed monochromators, thereby avoiding any moving parts.
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Fast, All-in-One Testing for Sulphur, Nitrogen, Halides
The Antek MultiTek™ by PAC (USA) is the testing system for fast, accurate detection of sulphur, nitrogen, and halides. MultiTek™ is the only instrument on the market that combines testing for sulphur, nitrogen, and halides all in one. It is compact, powerful, automated, and multi- configurable, it’s the perfect solution to today’s increasing demand worldwide for fast, accurate detection and analysis of unwanted chemicals, pollutants, contaminants, and corrosive elements. MultiTek™ delivers precise results with high sensitivity and unmatched versatility.
MultiTek™ detects sulphur, nitrogen, and halides through a uniquely efficient process that includes
combustion Ion Chromatography (IC), Ultraviolet Fluorescence (UVF), and
Chemiluminescence technologies. MultiTek™ is superior to wet chemistry and XRF; works with solid, liquid, gas, and LPG samples; and provides lower detection levels than competitive systems.
MultiTek™ helps users protect electronics, refinery products, and others against the corrosive effects of halides (Chloride, Fluoride, and Bromide) and Sulphur; protect people, animals, plant and aquatic life from the harmful effects of Halides, Sulphur, and Nitrogen in the environment. MultiTek™ also helps users reduce overhead costs, increase productivity, and ensure product compliance across a wide range of industries and applications, from fuels to pharmaceuticals to‘green’ manufacturing. MultiTek™ is part of PAC’s well-established Antek product line.
Reader Reply Card No 86 February / March 2011 •
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Complete Range of Certified Standards
Horiba Scientific is supplying its own range of standards as well as Spex CertPrep standards. In consequence Horiba Scientific proposes a complete range of Certified Standards Samples specifically for Sulphur in Oil analysis, as well as many other components in all kind of hydrocarbon matrices.
The three basic sets are dedicated to the most famous analytical methods of sulfur in oil analysis. The calibration is very simple and reliable. It is available from stock for ultra quick delivery, selectable individually or by set; S in heavy Oil, set of 8 Stan- dards from Blank up to 4%S - recommended for XRF: ASTM D4294 / ASTM D2622 / ISO 20 847; S in Base Oil, set of 14 standards from blank up to 1000 ppm S - recommended also for XRF, but mainly for UVF: ASTM D5453 / ISO 20 846; and S in Diesel Oil, set of 15 standards from blank up to 1000 ppm S - recommended mainly for UVF.
When the above range of product is not suitable for your application, Horiba Scientific proposes certified Custom Standards from Spex CertiPrep, which will totally match your requirements. You select the matrix, including any kind of Bio fuel, the elements and their concentrations for your standard and it will be made specially and delivered with certificate of analysis. For high quality results, this is the ideal solution to be sure you are always using the standards, which match the best your sample.
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