Analytical Instrumentation 37
High Resolution, Cryogen-Free NMR at a Fraction of the Cost
Oxford Instruments (UK), one of the world’s specialist NMR specialists, has launched Pulsar - an affordable benchtop, cryogen-free NMR spectrometer that offers convenience without the special requirements and cost associated with superconducting magnets.
Pulsar offers performance without expensive liquid helium, making it suitable for virtually any chemistry laboratory and ideal for teaching NMR to undergraduates. Professor David Haddleton in the Department of Chemistry, University of Warwick, UK has been trialling Pulsar in his undergraduate laboratory.
“Pulsar was introduced into a year three synthetic chemistry undergraduate laboratory at Warwick and used to follow real time organic, inorganic and polymer reactions taken direct from the reaction medium. Installation was simply plugging in the 13A plug and leaving to warm up overnight”, says Professor Haddleton. “The absence of the requirement for deuterated solvents and the ability to collect excellent quality FT NMR in a single pulse in less than 2 minutes with instant exportation into all NMR software was incredibly valuable for our students. The experiment was easier and quicker than a TLC (Thin Layer Chromatography) with massively more information. The instant availability of the data proved invaluable for the selection of experiments required on the standard high field NMR spectrometer, thus freeing up instrument time and greatly reducing the need for time on more expensive instrumentation. This is a must for undergraduate laboratories and research laboratories without access to high field instrumentation.”
Pulsar requires a standard mains electrical supply and is offered at a fraction of the selling price of current high field NMR instruments with virtually no on-going running costs. It incorporates a 1.4T (60MHz proton resonance) rare-earth permanent magnet with superior homogeneity, providing outstanding spectral resolution, generating routine spectra in seconds. Instrument control comes from a seamless workflow package, while the processing and manipulation of data is achieved using the industry-leading Mnova NMR software from Mestrelab.
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Analysis of Sulphur and Chlorine in Crude Oil by EDXRF
Applied Rigaku Technologies, Inc. (USA) has published a new application note describing the analysis of sulphur (S) and chlorine (Cl) in crude oil by energy dispersive X-ray fluorescence (EDXRF). The report includes complete information about sample preparation, method calibration and repeatability, and demonstrates the multi-element capabilities of the new Rigaku NEX QC+ analyser.
EDXRF is a technique widely used in the industry for sulphur measurement, as well as for measuring other elements present in oils and fuels. The analysis method described in the new report offers a fast, simple means of screening and monitoring the chlorine content of crude at the well site, along pipelines, during blending and other pre-refining examinations. For the analysis described in the report, eight certified oil standards were used to develop empirical calibrations for sulphur and chlorine. The empirical method
was used to determine the detection limits for both elements. Measurements shown in the report were carried out on the Rigaku NEX QC+ spectrometer, a new low cost, high resolution benchtop EDXRF elemental analyser featuring a high-resolution Peltier cooled Silicon Drift Detector (SDD) and 50 kV X-ray tube, which provides greater applications versatility and low limits-of-detection (LOD). The configuration is designed to enable more precise analytical results with shorter measurement times.
The results demonstrate that, given stable samples, proper sample handling and proper calibration techniques, the use of compact benchtop instrumentation employing semiconductor detectors can easily resolve and measure sulphur and chlorine present in oil. The spectrum presented confirms that the Rigaku NEX QC+ EDXRF analyser can achieve excellent results in screening and monitoring the concentration of sulphur, chlorine and other elements in crude oil and other similar oils.
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