This article was published in LABinsights www.labinsights.net ©maXus media ANALYTICAL INSTRUMENTATION Chemical Engineer David Kasius analyzes biodiesel for Fatty Acid Methyl Esters using the DVSL FAME analyzer. Mark van Andel, Lab Manager at Bureau Veritas on Fatty Acid Methyl Ester analyses in biodiesel ‘It’s great to have FAME equipment delivered ready to use’ As the use of biodiesel increases, so does the importance of Fatty Acid Methyl Ester (FAME) analyses. A year ago, Bureau Veritas’ Amterdam lab invested in special equipment to quickly analyze FAME samples from ship cargoes. Text: Els van den Brink | Translation: Word’s Worth | Photography: FOODnote Bureau Veritas’ laboratory in the Port of Amsterdam speci- alizes in analyzing gasoline, diesel, fuel oil and aviation fuel. Not far from the lab, tankers carrying shipments of these fuels navigate the North Sea Canal. No ship is allowed to load or unload its cargo until the fuel quality has been checked by an independent laboratory. Which is why Bureau Veritas has a team of analysts on standby 24-7. They check samples and deliver their quality control results as fast as possible. Their tests include density measurements, fuel composition and octane or cetane number. October 2019 | LABinsights 1 This article was published in LABinsights www.labinsights.net ©maXus media ANALYTICAL INSTRUMENTATION ANALYTICAL INSTRUMENTATION W Lab Manager Mark van Andel at Bureau Veritas in Amsterdam: “We got the FAME analyzer actually ready to use. All we needed to do was validate it.” T David Kasius checks the results of the FAME analysis. In 2010, the Amsterdam lab, formerly known as Inspectorate, became part of Bureau Veritas, a global company specialized in commodity inspections and analysis with over 600 offices and laboratories in more than 140 countries. In the Netherlands, ‘Next year, 10 percent of all fuels must be renewable’ Bureau Veritas has labs in Amsterdam, Rotterdam, Amersfoort, Vlissingen, Dordrecht, Botlek and Europoort. Biodiesel The lab is home to assorted flasks of gasoline and black fuel oil, interspersed with flasks and jerrycans filled with biodiesel in different shades of yellow. “The exact color depends on what the biodiesel is made out of, for instance, rapeseed oil or deep- frying fats,” says Mark van Andel, Lab Manager at Bureau Veritas Amsterdam. In accordance with EU law, 10 percent of all fuel must be renewable by 2020. This target is achieved mainly by adding biofuel to regular diesel and gasoline and slowly incre- asing that percentage, so that the automotive industry has a chance to adapt their car engines to this changing composition. Currently, diesel is called B7, which means that it contains a maximum of 7 percent biofuel. Two-step production Biodiesel must be checked for glycerides and methanol. That is because regular biodiesel consists of fatty acid methyl esters (or FAME), produced from vegetable oils or animal fat. This is a two-step process. Using a base—usually potassium hydroxide—the triglycerides in the oil are first converted to glycerol and free fatty acids. Using methanol, these fatty acids are then esterified into fatty acid methyl esters. Because both steps are equilibrium reactions, there is no complete conversion. That’s why it’s important to purify the fatty acid methyl esters. Any remaining glycerides could clog up the engine and cause additional soot when burned. Methanol is another undesirable byproduct, because it is toxic and can cause emission of harmful aldehydes. This is why biodiesel is checked so thoroughly for glycerides and methanol. Triple analysis To keep up with the growing importance of biodiesel, Bureau Veritas Amsterdam started analyzing FAME in September 2018. Its FAME analyses include three tests that are intended to detect specific characteristics of the FAMES: their fatty acid compo- sition, methanol content, and glyceride content. Using custom developed equipment, Bureau Veritas is able to perform these analyses largely automatically. Its GC analysis is done by a FAME analyzer developed by Da Vinci Laboratory Solutions based on ‘All we needed to do was validate the analyzer with our own materials’ Agilent equipment, Van Andel explains. “It uses a polar column, a flame ionization detector and an autosampler.” Although there are three analyses, only two gas chromatography columns are deployed. “We can use the same column with two different auto- samplers to run the MC analysis and the fatty acid analysis,” says Van Andel. “To determine the fatty acid composition, a liquid sample is injected. To measure the methanol content, the sample is heated, causing the methanol to evaporate. The evaporate is then sampled.” Manual sample prep The analyses are not fully automated, but that’s not necessary either, says Van Andel. “We don’t run these tests back-to-back all day long. That’s why we do sample prep manually.” This is relevant in particular for the glyceride content determination, which detects glycerol and mono, di and triglycerides. These substances have a relatively high boiling point, which means they have to be silanized beforehand: a reagent—MSTFA: N-Tri- methylsilyl-N-methyl trifluoroacetamide—is added to lower the glycerides’ boiling point. Turn-key delivery Van Andel was happiest with the fact that the FAME equipment was delivered ready for use. “This enabled us to start using it right away. Usually when you buy a piece of equipment, you first have to set up a method, find out what the best settings are, calibrate the instrument, measure various standards, and validate the instrument with certified reference material. This can easily take a few months. This time we got the instrument and it was actually ready to use. All we needed to do was validate it with our own materials and we were good to go!” Even more accurate The accuracy of FAME analyses will only continue to grow, Van Andel predicts. “The measurements are getting ever more accurate and reproducible. That’s partly due to the new NEN standard, EN 14103:2018, which is being drafted now. The old standard, from 2011, allowed a 4 percent variation, which is actually quite a lot.” In the new standard, that percentage is going to be reduced to 2.5 percent. The software in the DaVinci FAME analyzer is already prepared for this change and takes into account the fact that the various FAMES do not all produce the exact same response in the detector, even when the same amount is injected. This can be addressed by assigning each type of FAME a specific response factor in the calculation. 2 LABinsights | October 2019 October 2019 | LABinsights 3 More information on this technique via www.davinci-ls.com/en/contact/contact-head-offifices

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