Analytical Instrumentation 29
Table 3: Sulphur concentration corresponding to the injection of 6 loops of 100 µl butane LPG of an unknown concentration.
Table 2: Sulphur concentrations resulting from UV fluorescence-based detection of SO2 following complete combustion of known quantities of sulphur-containing butane LPG in the iPRO 5000 S
analyser.
Figure 2 shows typical peak shapes arising from the injection of three repetitions of four loops of thiophene-bearing butane LPG. The thiophene content was 10.15 mg/kg, corresponding to a sulphur content of 3.8 mg/kg. The high degree of reproducibility was typical of the measurements and is consistent with the low RSDs presented in table 2 and table 3. Finally, a sample of LPG with unknown concentration was analysed for sulphur content using the calibration data presented in figure 1. The results of the analysis are presented in table 3 and reveal the sulphur content to be 23.36 mg/kg
Conclusion
Natural gases such as LPG are increasingly being used as fuel feedstocks for a variety of fuel cell technologies and applications. Fuel cells and the reformer catalysts are generally not sulphur tolerant and, depending on the technology employed, sulphur can cause contamination and degradation of power generation performance. The need for low-level sulphur measurement in the fuel cell industry will continue to grow as various technologies see wider deployment of LPG and emission reduction targets become increasingly tougher.
Emerging technology has overcome the requirement to use two introduction modules for the precise analysis of sulphur in light and heavy hydrocarbons, offering a new design of injector module that improves the accuracy and precision of results, while reducing analysis time to within three minutes compared to the boat inlet method which took twelve minutes. In addition, these systems can determine the sulphur content of common middle distillates by direct spray injection using UV fluorescence in accordance with ASTM D6667. Experimental results indicate that this technique analyses sulphur content with high precision and accuracy.
References
[1] ASTM D6667 Standard Test Method for Determination of Total Volatile Sulphur in Gaseous Hydrocarbons and Liquefied Petroleum Gases by Ultraviolet Fluorescence
Figure 2: Peak shapes arising from the injection of three repetitions of four loops of thiophene- bearing butane LPG. The thiophene content was 10.15 mg/kg, corresponding to a sulphur content of 3.8 mg/kg. The high degree of reproducibility was typical of the measurements and is consistent with the low RSDs presented in table 2 and table 3.
[2] Regulatory Impact Analysis: Heavy-Duty Engine and Vehicle Standards and Highway Diesel Fuel Sulphur Control Requirements—EPA420-R-00-026 (2000); United States Environmental Protection Agency.
For more information about the Thermo Scientific iPRO 5000 series analyser, please call +1 800- 532-4752, email
analyze@thermofisher.com or visit
www.thermoscientific.com/ipro
CNS SIMDIS Introduced for Crude Oil Analyser
PAC (USA), a global provider of advanced analytical instruments for laboratories and online process applications, announces the introduction of the AC Analytical Controls CNS SIMDIS for Crude Oil analyser. It is the first instrument on the market to simultaneously determine the boiling range distribution of Carbon, Nitrogen, and Sulphur in crudes and final products, which is essential to cutting the crude oil to optimise the manufactured end product. It is also able to analyse a wide variety of crude products, including everything from heavy gas oils to naphtha.
The CNS SIMDIS for Crude Oil is built around recognised simulated distillation (SIMDIS) methods, but also incorporates additional Chemiluminescence detectors. It is comparable to methods, such as ASTM D2887, D6352, D7500, and D7169 standards; however, it completes crudes assays at a fraction of the time and cost as the traditional methods.
Its integrated software automates several aspects of the analysis process, including calibration, validation, and data reporting. With no prior software experience needed, the CNS SIMDIS for Crude Oil is easy to use and also provides extensive reporting capabilities.
“Even though analysing crude assays is essential to refinery profitability, traditionally, it has been a time consuming and difficult process. We at PAC recognised this gap and wanted to introduce an instrument to the market that made crude assays simple to perform,” said Daniel Benitez, PAC Vice-President Product Management. “By delivering an assay within 30 minutes, the CNS SIMDIS for Crude Oil provides an excellent tool to optimise crude oil blend processed in the refinery.”
Reader Reply Card No 67 Elemental Analysis by Combustion
By incorporating state-of-the-art hardware and software technology with key improvements in overall instrument performance and reliability, the CHN628 Series from LECO Corporation (USA) makes it possible to achieve fast results in organic matrices from food to fuels.
For optimum versatility, this instrument is available in flexible configurations—nitrogen/protein, carbon/nitrogen, and carbon/hydrogen/nitrogen. An optional sulphur add-on module provides independent sulphur determination for macro samples up to 350 mg in less than two minutes. An optional liquid autosampler provides seamless operation for liquid sample analysis up to 1 mL. An oxygen add-on module for micro oxygen capabilities is also now available.
The CHN628 Series incorporates features designed to maximise throughput while keeping cost-per-analysis low. The unique combustion
gas-handling and aliquot dosing system significantly extends the lifetime of the reagents used, eliminating the need for chromatographic separation techniques and other costly whole-gas analyses. A simple, gravity-fed autoloader allows for unattended analysis, while increasing long-term reliability of the loader. Independent detectors are used for simultaneous elemental determination, resulting in rapid analysis times.
For the operator, the instrument provides enhanced accessibility and ease-of-use. For safety and convenience, reagent and reduction tubes are located on the front side of the instrument behind the cabinet door, along with specially designed tools and storage to aid in performing maintenance tasks. The easy-to-use CHN628 software offers simplified data handling, customisable data reporting and exporting, and a number of user-defined settings, all with tools for compliance to FDA regulations 21 CFR Part 11 for a closed analytical system.
Reader Reply Card No 68
i-Fischer Engineering GmbH Dachdeckerstr. 1 97297 Waldbüttelbrunn Germany
Tel: +49 / [0] 9 31 / 46797-0 Fax: +49 / [0] 9 31 / 46797-29 web:
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expect essentials
Reader Reply Card No 69 April / May 2012 •
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