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ANALYTICAL INSTRUMENTATION Distillation specialists give helping hand


to developing the green fuels of the future Reducing CO2


significant and should be achieved as quickly as possible.


Even with exploring more and more sources of fossil fuels, together with the allied technical improvements in extracting more products out of already existing wells, it is clear that the availability of mineral fuels will end one day and will require replacement by green fuels in order to keep the wheels of industry and commerce turning.


Governments around the globe have decided to lead their countries to a climate-neutral state in the future, in other words, the goal is “zero emissions”. In this regard, the use of well-established technologies with clean energy offer immediate answers. The combustion engine is a well-known technology and liquid-fuel is one of the energy sources with a significant energy density, easy to transport and store and with an already existing corresponding distribution.


The only challenge remaining is: what could be a plausible alternative “green fuel”?


The solutions are almost ready to be implemented: ILUDEST has participated in several projects at universities and research institutes in the field of these renewable energies. One of these alternative fuels is OME (Oxymethylenether) which burns with almost no carbon particles. The OME is produced in a reactor. During the reaction process several by-products, along with OME, are produced. To reach the quality of a Diesel substitute, the OME must be purified in a distillation unit with a high separation efficiency.


It does not take much to turn dreams into reality: tomorrow’s value chain is supposed to be climate-neutral, or at any rate sustainable, and preferably without the use of fossil raw materials. However, the technology that promises prosperity for all without environmental pollution is still a long way off. Today, no one disputes that it is possible in principle to produce fuels and basic chemicals from renewable energy and waste gases. However, these processes also must be economic. And so, institutes, companies and politicians seek the mythical ‘philosopher’s stone’ of instant success in chemical synthesis.


“The processes we need are actually already developed,” says someone who should know: Jakob Burger, Professor of Chemical and Thermal Process Engineering at the Technical University of Munich (TUM), is researching the direct synthesis of artificial fuels with his team at the TUM campus in Straubing, in Germany. The means equipment required is a reactor about the size of a table, plus distillation columns several metres high and a downstream membrane unit. This is a typical pilot plant set-up—but very robust and one that packs a significant punch!


ILUDEST designed and manufactured the distillation modules, comprising two towers, one in glass for operation under vacuum, and a second in stainless steel for operation under overpressure.


Alternative fuels contain several short-chained molecules with very low boiling points. These short-chained molecules must be separated, but separation of these products normally requires very low operating temperatures. Low temperatures can be reached by using expensive cryostats, but another way is to increase the operational pressure of the system. This leads to higher throughputs at the same column diameter compared to atmospheric pressure. The critical point of the products, the possibility to fill and drain the system, as well as pressure equipment directive and explosion proof design must be considered. Pressure distillation units can be realized in stainless steel or special materials, like Hastelloy.


Separation of alternative fuels has also been investigated in a multiple dividing wall column. Inside the column the ascending vapour stream can be separated into two separate parallel working columns. The backflow of one column can be separated as well into two columns.


All customer’s enquiries do contain the challenge of combining high separation efficiency with low temperatures, respective pressurized equipment, including the challenge to fill and drain the system adequately.


Publications about further projects already effected are under preparation and will be brought to your attention once available. More information online: ilmt.co/PL/vY3A


Removing the challenges of blank values and side reactions


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To combat this problem, an external oven is used. The industry standard is a “Headspace” oven, in which the sample is heated in a sealed vial until the water is extracted and carried directly into the titration vessel via a dry carrier gas, usually Nitrogen. Upon entering the vessel, the sample is titrated, without the addition of any additives or mercaptans. Although the Headspace technique combats the issues of side reactions, it is not without its own problems. A blank value for each empty vial is required. Quite simply, this is a measurement of the atmospheric moisture or water inside the empty vial. Depending on the size and storage conditions, a blank vial could contain anywhere between 30-80 micrograms of water. The blank value of each vial will change throughout the day, regular blank value checks are recommended. When using a detection technique as sensitive as coulometric Karl Fischer titration, these blank values simply do not provide true ppm accuracy.


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Take insulating oils for example, these have a water content of approximately 10ppm. Having a blank value which could be 3-8 times greater means you simply cannot rely on the result, and in many cases, instruments will display 0ppm as they cannot distinguish the true water content over the blank value content as the differential value is so small. Additionally, a problem associated with an external carrier gas is the fact that the system is regarded as “open”, meaning the methanol in the Karl Fischer solvent quickly evaporates causing immediate instability.


ECH Elektrochemie Halle have addressed all the above issues with the closed loop oil evaporator, which is available on the new Aquamax KF Pro Oil system.


Tom Gallant, of ECH Elektrochemie Halle explains how the Aquamax KF Pro Oil is the leading technology in the titration industry: “The oven is connected directly to the titration vessel via a pump and tubing which circulates the carrier gas in a “closed loop”. The sample is injected from your sample syringe directly into the oven, removing the requirement of a blank value, whilst containing the methanol meaning we can analyse over 1000+ samples without changing the reagent….All this, and just like the Headspace technique, all side reactions are eliminated. The Aquamax KF Pro Oil truly combines the best of both methods. The ECH closed loop principle on the Aquamax KF Pro Oil ensures true 1ppm accuracy, the longest reagent life and with our patented temperature gradient program you can clearly identify the free water and the chemically bonded water in your sample, creating a true research & development tool allowing you to know everything about the water in your fuels and oils.”


More information online: ilmt.co/PL/QG9J For More Info, email:


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49068pr@reply-direct.com 56429pr@reply-direct.com


Restek’s new D3606 column set achieves accurate quantification of toluene and benzene—including benzene in gasoline containing ethanol or butanol blends— with no compromising coelutions. An updated formulation with improved support material and polymers enhances robustness and reproducibility.


Listed in the ASTM Method D3606, Restek’s new D3606 column set helps labs attain better separation of benzene and ethanol while following ASTM method requirements. Restek’s two-column sets (cat.# 83606A) are individually tested for D3606 method applicability and include a QC test chromatogram with approximate backflush times.


More information online: ilmt.co/PL/ArBB For More Info, email:


using the new Aquamax KF Pro Oil for ppm water in oil and fuels There are a number of problems which have been identified when titrating oil and fuel samples via direct injection coupled with the coulometric Karl Fischer method. Additives used in lubricating oils and fuels, plus mercaptans in crude oils are known to cause detrimental side reactions when the sample is injected directly into the titration solvent, primarily resulting in lack of reproducibility and a breakdown of the solvents.


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55780pr@reply-direct.com emissions is an important current objective in reducing global warming. The scale and scope of this reduction of CO2 emissions needs to be


Reliably resolve benzene and toluene with new column set


ppm Water in Oils and Fuels Coulometric Karl Fischer Titrator


• 1000+ measurements without changing reagents • Eliminates all side reactions and no blank value


Cont act us to find out more on +44 (0) 1525 404747 or email info@echscientific.com


Fully automated Lab, Online and Portable system


WWW.PETRO-ONLINE.COM www.aquamaxkf.com


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