26 Report on Benchtop NMR System use at the BAM Federal Institute for Materials Research and Testing
The BAM Federal Institute for Materials Research and Testing operates under the guideline ‘Safety in Technology and Chemistry’. This defines tasks with the main emphasis on development and provision of CRMs, development and validation of complex analytical methods, methods for the assessment of analytical laboratories, and establishing and fostering national and international networks committed to the assurance of quality, reliability and comparability in analytical chemistry.
Dr Michael Maiwald and his colleague, Nicolai Zientek, MSc, use NMR in their daily research and development work. They use a high frequency 500 MHz online NMR spectrometer as their reference instrument. They ‘hyphenate’ NMR with conventional online analytical techniques such as NIR, Raman, UV/VIS spectroscopy and, in particular, medium resolution NMR spectroscopy. As Dr Maiwald said: “Our aim is to develop techniques to bring the benchtop lab instruments ‘into the plant’ and to show (in projects) how MR NMR could already be used for technical applications like online reaction monitoring. This led us to the acquisition of the Spinsolve Benchtop NMR spectrometer from Magritek.”
Asked why his group selected to use the Spinsolve, Dr Maiwald said: “We were impressed with the spectra – the symmetrical line shape and narrow line width was achieved even in technical mixtures. This is due to the use of Halbach magnets. The stability we observed over a given period of time without preparing the instruments was extremely good. We have seen that the Spinsolve remains working in specification for as much as 48 h in a technical environment. Pre-magnetisation below the active region of the magnet is important to us for online measurements. As far as we see, the instrument meets this requirement.”
Describing the projects to date, Dr Maiwald, said he has used the Spinsolve for flow-through reaction monitoring experiments. These have included the simultaneous observation of 1H and 19F in an esterification reaction. This was observed within 1/16” FEP tubing using a 5 mm outer diameter Dewar insert to keep the elevated reaction temperature. Looking ahead, Dr Maiwald and his group are planning to further improve online reaction monitoring with medium resolution NMR spectroscopy and develop automated data preparation and data analysis tools by developing chemometrics and automated signal processing tools.
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Eliminate Tedious Sample Preparation with Laboratory Automation
Supreme Performance and Accuracy for Infrared Analysis
Shimadzu’s middle class Fourier Transform Infrared Spectrophotometer, IRTracer-100, analyses materials quickly and easily in a variety of fields such as pharmaceuticals, food, chemicals and electronics, and monitors high speed reactions within a few seconds.
Compared to the well-reputed predecessor model, IRPrestige-21, the easy-to- operate IRTracer-100 features highly improved sensitivity, resolution and scan speed with expandability and easy maintenance. IRTracer-100 can quickly and easily obtain high quality data of small samples through 1.5-times higher sensitivity and high speed scanning of 20 spectra/sec.
IRTracer-100 achieves 60,000:1 SNR (signal-to-noise ratio) with improved interferometer and detector, and high speed reaction monitoring function for these demands. Combining with the LabSolutions IR Contaminant analysis program makes analysis of small samples easier, quicker and more accurate. LabSolutions IR on IRTracer-100 can be connected to Network system with LabSolutions software for LC/GC, and unifies management of obtained data and users to access the systems for pharmaceuticals demands.
IRTracer-100 can quickly and easily obtain high quality data of small samples from 1mm to 10µm. LabSolutions IR analysis program achieves results within a few seconds – compared to one hour duration using conventional means. IRTracer-100 also obtains high quality spectra of ppm-order additives and identifies them easily.
Shimadzu’s predecessor model IRPrestige-21 recorded spectra every 5 seconds, but the IRTracer-100 can obtain 20 spectra in a second in rapid scan mode (option). IRTracer-100 precisely monitors high-speed reactions such as curing of UV curable resin.
LabSolutions IR on IRTracer-100 enables connection to other laboratory hardware, for example LC and GC systems, and unifies management of obtained data. The number of spectra in standard IR libraries has been expanded from 1,000 to 12,000, and identification of unknown samples can be done with the standard system. The unique Easy Macro program supports easy-to-use operation, even by less- experienced operators.
Tecan offers a wide range of laboratory automation solutions for mass spectrometry (MS) sample preparation, ensuring there is a system to meet your workflow and throughput needs. From solid phase extraction and liquid- liquid extraction to protein precipitation and straightforward ‘dilute and shoot’ methods, Tecan provides seamless automation of routine sample preparation applications, helping to alleviate major bottlenecks for many laboratories.
Recent advances in MS instrumentation have led to an increasing number of laboratories choosing this technology for a wide range of applications. However, sample preparation techniques have not enjoyed the same rate of development, leading to processing bottlenecks and reducing overall productivity. Automation of routine sample preparation can alleviate these problems, reducing hands- on time and increasing throughput. With a broad base of MS customers in drug discovery, clinical, toxicological, food and environmental laboratories, Tecan is perfectly placed to deliver innovative automated sample preparation solutions for virtually any application.
Tecan offers an extensive range of systems and modules to match your laboratory workflow needs; from straightforward ‘pipette and shake’ sample extraction using the recently launched AC Extraction Plate™* to walkaway automation with a modular Freedom EVO®
workstation. Dr Stefan
Traeger, Head of Tecan’s Life Sciences Business, commented: “We are committed to helping our MS customers maximise their laboratory output. Advanced process security and sample tracking options, together with user-oriented features such as the TouchTools™ graphical interface, are making safe and reliable automated sample preparation easier than ever before.”
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Product Portfolio Expanded with Launch of ICP-OES PQ 9000 its first High-Resolution Array ICP OES (optical emission
Within its core segment for analysis measuring technology, Analytik Jena AG now offers with the PlasmaQuant®
spectrometry using inductively coupled plasma) for multiple element analysis as part of its own technology portfolio. This method is routinely used for determining smallest element concentrations especially in environmental analysis, material research, metal or pharmaceutical industries.
“The PlasmaQuant® PQ 9000 has been developed to master the most complicated analytical
challenges in emission spectroscopy with the highest degree of precision, method flexibility and operating comfort. In doing so, we are building on our longstanding experience in the development of high-end spectrometers,” said Torsten Olschewski, Head of the Analytical Instrumentation business unit at Analytik Jena AG.
Technological advances in the product include the optical resolution, the plasma torch design and the generation and observation of the plasma.
PlasmaQuant® PQ 9000 offers: clever bench-top design; innovative high-end technology;
impressive analytical performance; high sample efficiency; benchmark-setting operating comfort; premium quality ‘Made in Germany’.
PQ 9000 also allows for the safe analysis of rare earth metals such as cerium, lanthanum, neodymium or samarium in silicate-containing minerals. The high salt contents in these minerals (silicates) are not a problem thanks to the technology of the PlasmaQuant®
The PlasmaQuant®
PQ 9000 system. Spectral interferences caused by the high contents of these samples of main group elements such as sodium, aluminium or silicon can be detected with the help of high resolution and easily corrected.
Another application is the analysis of biodiesel for traces of metals such as sodium, potassium or manganese. These lead to foaming of the fuel and thus to unstable or lower performance as well as clogging of filters. Other trace elements to be controlled are phosphorus and sulphur, which are known as catalyst poisons. In addition, the sulphur r dioxide produced during combustion is an environmental pollutant.
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INTERNATIONAL LABMATE - APRIL 2014
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