ASTM D7039. Sulfur analysis plus a further 21 elements by MWDXRF. Model SS1000-S Sulfur in oil, petrol, diesel All liquids The new S1000 series MWDXRF
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1 Spectrolab Science cat71120p Sulfur analysis plus a further 21 elements by MWDXRF Model SS1000-S Sulfur in oil, petrol, diesel All liquids The new S1000 series MWDXRF ASTM D7039 and other standards For ultra low levels of Sulfur in fuels LOD 0.2ppm The need for lower detection methods of Sulfur in hydrocarbon fuels In order to reduce the harmful emissions of pollutants such as sulphur and its derivatives in the environment, stricter quality standards for hydrocarbon fuels are now in place. The limit of Sulfur content in gasoline has been reduced from 150 ppm to 10 ppm and further restrictions will shortly apply to the level of 1 ppm or lower. Standard XRF technology does not work well at this level due to interferences within the measurement and low overall sensitivity. For this reason there is a need to revise testing methods and instrumentation. These changes can be found in the V and IV vehicle fuel standards, which have been introduced in ASTM D7039 "Standard Test Method for Sulfur in Gasoline, Diesel Fuel, Jet Fuel, Kerosene, Biodiesel, Biodiesel Blends and Gasoline-Ethanol Blends. There are several options that can provide enhanced sensitivity. The preferred analytical method is Monochromatic Wavelength Dispersive X -ray Fluorescence Spectrometry MWDXRF Based on the method of monochromatic wavelength dispersive X-ray fluorescence spectrometry (MWDXRF) the new SS1000-S series X-ray fluorescence spectrometer is the perfect instrument for determining ultra-low sulfur content, offering the advantages of high sensitivity detection, excellent descrimination and fast analytical times. The SS 1000_S X-ray fluorescence spectrometer can be used for the production and quality control required in oil refining and petrochemical oil storage or transportation. Also oil and fuel quality supervision in government departments, military and many other similar applications. The SS 1000-S is a compact desk top analyser able to measure the concentration of Sulfur in fuels such as gasoline, diesel, petrol, aviation fuels, kerosene, biodiesel and biodiesel blends as well as gasoline-ethonol blends, etc at the sub ppm level and at high speed. Chlorine options with similar LOD s are also available
2 How does the new technology work Conventional XRF systems currently used for Sulfur analysis are based on a simple Xray source collimated by a pin hole aparture. Polychromatic Xrays illuminate the sample and any fluorescence is detected using a conventional silicon detector. The resulting signal is then energy descriminated and processed. The problem being that the pin hole collimators and filters used, significantly reduce the number of photons at the sample and discrimination is incomplete. This new technology described as MWDXRF overcomes these design limitations in a number of ways avoiding the need for pin hole collimators and filters. In addition interferences are also eliminated. With MWDXRF incident X-rays are generated by a microfocus X-ray source and focussed onto the sample using a Johannson monochromatic focussing mirror. Secondary X- rays diffracted by the sample are then focussed by a second Johannson monochromatic mirror onto a detector. This arrangement provides for extremely low backgrounds with the advantage of simple or no matrix corrections. The Secondary focused X-rays onto the detector are practically free from spurious background effects and most other sourcers of unwanted radiation which normaly limit the performance of coinventional EDX and WDXRF The result being an analyser capable of extremely high sensitivity, LOD s of 0.2ppm and superb S:N ratios Features Compact desk top lab instrument or can be used as an on line analyser Offers high reliability and requires no routine service An advantage of this type of spectrometer is that it is inherently simple in concept. There are no moving parts to go wrong. All optics are carefully adjusted at the factory for optimum performance and locked into position. Installation is simply a matter of switching the instrument on and checking performance relative to normal standards as supplied All electronics are state of the art employing a unique digital shaping MCA and a digital pulse height analyser with features that include fast baseline restoration and optimum peak detection Convenient automatic drift correction can be checked using simple solid samples with high, medium and low concentrations Calibration curves are pre installed according to order allowing accurate analysis in all matrixes including petrol, diesel and aviation fuels. Additional calibration curves can easily be configured as required. Applications Gasoline, Diesel, Jet fuel, Kerosene, Biodiesel and blends, Gasoline Ethanol blends Source Johansson type focussing monochromatic mirror
3 . ẹ- Primary o u t p u t spectrum Spectrum of DCC Monochromatic excitation: e- 'ii,[ n I! I! " ".....!!.!! Energy KeV II Energy KeV "'" Spectrum of ultra low Chlorine concentration ppm lppm II,~ " H U Energy KeV).. Primary output spectrum of Cr target X-ray tube. The intensity of Cr K alpha line is about 30% of total emission Note 1 Johansson type DCC focussing optics are designed only to capture a narrow bandwidth of Xrays from the source and focus the Xray beam into a small spot which then illuminates the sample. The DCC is also monochromatic allowing only discrete radiation to become incident on the sample ensuring extremely low background levels. A Spectrum of monochromatic excitation. The S:N background is significantly improved using monochromatic excitation of the Cr K alpha line Note 2 A state of the art energy dispersive detector is employed along with the Johansson focussing monochromator in order to eliminate any unwanted radiation and so ensuring the best possible S:N ratios making ultra low detection possible A Spectrum of ultra low Chlorineconcentration is directly proportional to Chlorinecontent Note 3 By eliminating the need for pin hole collimators the intensity of Xray rays is substantially increased in some cases by as much as X100. This means that low power Xray sources can be employed and which provide for higher Xray flux providing an overall increase inl sensitivity and S:N Johansson type optics are the state of the art for XRF anaalysis The unique optical design has no moving parts and alignment is factory set. There are no moving filters or collimators. This makes installation extremely simple and is esstentially plug and Play It also means that there is no service requirement
4 The unique SS100-S Sulfur MWDXRF analyser Specifications LOD 0.2ppm S (300 S) RANGE 0.45ppm-2% TIME 60S-300S(USER SELECTABLE) REPEATABILITY Sn ppm(2 ppm),0.5 ppm(10 ppm) STANDARDS ASTM D7039 ISO15597 VOLUME 614 mm (W) 444 mm (D) 375 mm (H) POWER (110±10)VAC, 5A;(220±20)VAC, 5A OUTPUT INTERFACE USB OPERATING TEMPERATURE 10 ~35 X-ray source Elements Chromium target Optics Hardware Software Microfocus spot focus 175um Sulfur plus 21 elements Be window 10um Johannson monochromatic focussing mirrors High speed processor on embedded system platform Touch pad with graphical user interface Calibration, drift correction, data browse, statistics Data collection and processing, print. APPLICATIONS Analysis of ultra-low Sulfur content in gasoline, diesel, naphtha and aromatic hydrocarbons - Single-wavelength dispersive X-ray fluorescence spectrometer with ultra-low detection limit The detection of chlorine content in refined oils and intermediate products is an important indicator. S2000 is easy and accurate to detect ultra-low chlorine content in gasoline, diesel, naphtha and aromatics. Analysis of trace Sulfur content in residue
5 Specifications X-ray source Microfocus spot focus 175um Elements Sulfur plus 21 elements Chromium target Be window 10um Optics Johannson monochromatic focussing mirrors Hardware High speed processor on embedded system platform Touch pad with graphical user interface Software Calibration, drift correction, data browse, statistics Data collection and processing, print. Limits of detection 0.2ppm sulphur in fuel Range 0.2ppm 10% Time 30 to 300 Secs Power V 500W Oxford House, 20 Oxford St. Newbury, Berkshire. RG14 1JB UK. Offices in UK, EU, Dubai Our partners in EDXRF Ametek,Anchor Wisdom Tech, Anaspec, Hitek cat71120
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