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Major investments are often made in state-of-the-art XRF equipment without knowing that the whole analytical chain, including the weighing step in sample preparation prior to fusion, is of crucial importance to get precise and accurate analytical results and consequently obtain estimated financial pay-offs. In fact, precision and accuracy of results enable the manufacturer to decrease the level of uncertainty associated with the concentrations of its products, and therefore avoid huge losses in revenue. The weighing step in sample preparation by fusion for XRF analysis is all about knowing the exact weights of the sample and the flux (sample-to-flux ratio). Consequently, the weighing method, the tolerance accepted as well as the analytical method to obtain this ratio will affect the quality of analytical results given by the spectrometer. There are many ways to weigh the sample and the flux prior to fusion: • Manual weighing (most widespread technique) • Automated weighing (with Claisse® LeDoser™ or LeDoser-12™ for example) • Weighing the sample and the flux directly in the platinum (Pt) crucible • Weighing the sample or the flux in another container, reusable or not, before transferring it into the Pt crucible • Pre-weighed flux vials • Weight correction on the XRF instrument (exact weight needs to be known) All these weighing methods affect the precision of the sample-to-flux ratio and consequently impact the final analytical results. In this application note, the effect of the different weighing methods on the precision (RSD) of the obtained XRF results are compared.

Products:
Claisse range
Date:
January 10 2019
Language:
English
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Mining companies can lose millions of dollars if a slight bias is found in their whole ore analysis process. Their profitability then depends on the quality of their elemental analysis. This study shows that it is possible to use NaT flux coupled with an automatic fusion instrument to build a calibration strategy for XRF analysis that meets the ISO 9516-1 requirement for iron ore analysis. A calibration strategy based on CRMs prepared with NaT as flux is comparable to lithium-based flux for iron ore analysis. The developed method allows fast and repeatable analysis of iron ores in accordance with the currently accepted international norm. This method is a nice alternative to lithium-based flux used for sample preparation by fusion.

Products:
Claisse range
Date:
January 10 2019
Language:
English
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Malvern Panalytical has developed a novel approach for the reliable and consistent preparation of pressed powdered dairy samples. This approach minimizes heterogeneities, providing a truly representative sample and immobilizes the fat content allowing a unified pressing process, producing stable and consistent pressed pellets for a wide range of samples. This solution is valuable in a large number of industries including dairy product manufacturers, ingredient and food manufacturers, suppliers, analytical and research labs.

Products:
Epsilon 4
Date:
January 10 2019
Language:
English
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The morphology and chemical composition of complex powder mixtures are often Critical to Quality in pharmaceutical products. Component-specific particle size and shape information measured by the Morphologi 4-ID within a powder blend can help compare the physicochemical attributes of a generic (test) product with the reference listed drug (RLD) in order to establish pharmaceutical equivalence as part of a bioequivalence study, accelerating generic drug development. Here, we present an example case study of the use of MDRS to compare a generic oral solid dose cold and ‘flu product to the RLD, where both products are licensed from the same Marketing Authorization holder.

Products:
Morphologi 4-ID
Date:
December 5 2018
Language:
English
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Polyalfaolefins (PAO) are a range of low molecular weight hydrocarbons, used in a number of lubricant applications. In particular, they are widely used in the industrial and automotive industries where they are used as base oils. The wide functional temperature ranges, high oxidative stability and high viscosity indices all contribute to their desirable qualities. As with so many polymers, the specific physical properties of PAO are strongly determined by their molecular weights. As a polymer of decene, a PAO sample will likely be a mixture of different decene oligomers and polymers, thus the final molecular weight distribution of a PAO sample will depend on polymerization parameters. As a lubricant, the primary tool for characterizing PAO samples will be a viscosity or rheology measurement, however, gel-permeation/size-exclusion chromatography (GPC/SEC) can be used to make measurements of PAO molecular weight distribution, which may offer insight into small differences between samples. Historically, GPC has been a slow technique with measurements taking 30-60 minutes to separate the sample. Additionally, the molecular weight result is determined by comparison to polymer standards of different structure and chemistry, making the result only relative. Despite this, the technique is a powerful tool for comparing samples and has become the gold-standard of molecular weight measurement in the polymer industry. The addition of advanced detectors such as light scattering and a viscometer can help overcome some of the limitations of GPC. Light scattering allows for the direct measurement of the polymer’s molecular weight, independent of its structure or chemistry providing what is often referred to as absolute molecular weight. The use of a viscometer allows for the measurement of some structural aspects including branching. In the last few years, further developments in GPC column chemistry have resulted in the development of Advanced Polymer Chromatography (APC) systems. These use smaller particle sizes to achieve superior resolution but generate higher backpressure. This also offers the benefits of significantly reduced run-time and solvent use. Previously, the narrow peaks generated by APC were incompatible with multi-detection because of the effects of band-broadening (also called dispersion) caused by entry and exit of the detector cells. This has now been overcome and it is possible to combine multi-detection with APC with multi-detection to perform absolute characterization of polymers at the timescales and resolutions of APC. As low molecular weight molecules which are mixtures of oligomers, PAO, are an ideal example of this. In this application note, the separation of PAO by multi-detector GPC and APC are compared and the benefits of multi-detector APC are discussed.

Products:
OMNISEC system
Date:
December 5 2018
Language:
English
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