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Safe, automatic  solvent purification Quick, well-managed distillation at Radboud University
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Safe, automatic solvent purification

Quick, well-managed distillation at Radboud University

Purifying ultra dry solvents in a solvent purification system is quicker and safer than distilling them. PhD candidate Hidde Elferink at Radboud University’s faculty of Synthetic Organic Chemistry explains. “We research the chemical bonding of sugars, also known as glycosylation. We need extremely pure, dry solvents for that. When we used to distill those, things sometimes went wrong. Now, purification is fast, safe and flawless.”
Distillation is a great old-school method for drying solvents. But it is neither quick, nor easy, says Hidde Elferink. “I hated doing it when I was a student. Setting things up in the lab takes up so much time and space. So much can go wrong. Just take THF [tetrahydrofuran] for instance. If you don’t pay very close attention, it goes dry and then it can combust. I must admit that in my student days, I caused several fires and even a small explosion.”
www.labinsights.nl ©maXus media THEME: SAFETY Purifying ultra dry solvents in a solvent purification system is quicker and safer than distilling them. PhD candidate Hidde Elferink at Radboud University’s faculty of Synthetic Organic Chemistry explains. “We research the chemical bonding of sugars, also known as glycosylation. We need extremely pure, dry solvents for that. When we used to distill those, things sometimes went wrong. Now, purification is fast, safe and flawless.” Alinda Wolthuis | Photography: FOODnote Distillation is a great old-school method for drying solvents. But it is neither quick, nor easy, says Hidde Elferink. “I hated doing it when I was a student. Setting things up in the lab takes up so much time and space. So much can go wrong. Just take THF [tetrahydrofuran] for instance. If you don’t pay very close attention, it goes dry and then it can combust. I must admit that in my student days, I caused several fires and even a small explosion.” Ultra dry solvents Elferink works on sugar chemistry in a group led by Professor Floris Rutjes and Thomas Boltje. “Many of us are die-hard orga- LABinsights | February 202033 Quick, well-managed distillation at Radboud University Safe, automatic solvent purification When the tube is full of ultra dry toluene, it is capped with a stopper. There is no need to wear gloves when drawing the solvent, as lab workers will at no point come into contact with it. nic chemists,” says Elferink about himself and his colleagues. “In our group, we study sugars in and on cells. We work on methods for creating synthetic sugar trees that play a role in the communication between cells, for instance. That’s important for the development of vaccines and for understanding the immune system. In our work, we need ultra dry solvents to prevent unwanted side-reactions. During glycosylation, extremely reactive particles are formed, which need only a tiny amount of water to create a bond and ruin an experiment.” The research group dries solvents using a fully automated system called the MBraun Solvent Purification System, produced ‘The automated system is more controllable and safer because it releases no heat’ www.labinsights.nl ©maXus media The MBraun Solvent Purification System (MB SPS) was specifically developed for labs that need a safe, quick and easy method for dosing ultra dry solvents. The solvent purification system is fully automated. The solvent tanks are pressurized with inert gas (usually a nitrogen source that is at least 99.99% pure). The solvent rises through the dip tube and passes through a double filter column THEME: SAFETY PhD candidate Hidde Elferink of the faculty of Synthetic Organic Chemistry at Radboud University draws ultra dry solvent from the MBraun Solvent Purification System. The The MBraun Solvent Purification SystemMBraun Solvent Purification System that absorbs the moisture from the solvent. The ultra dry solvents are then dosed into receivers directly next to the system and/or in an integrated glovebox. That process is PLC-driven. Every line is regulated independently. Each system can accommodate seven solvent tanks. The lab is kept safe by a hazardous materials storage container for the flammable fluids. February 2020 | LABinsights 34 www.labinsights.nl ©maXus media THEME: SAFETY LABinsights | February 202035 by Salm en Kipp. “The process is really simple. We use five solvents: toluene, THF, dichloromethane, acetonitrile and diethyl ether. These solvents are stored in individual tanks and are then pumped up and led through a filtration system that removes most of the water. What remains is stored in nitrogen. That leaves you with very dry solvent. Basically, you have solvents ‘on draft’. It works perfectly. I have seldom experienced any hydrolysis side-reactions.” No distillation stress A single, 1.5-meter-wide system is enough to serve the 80 people that work in the lab. No one ever has to wait to use it, Elferink says. “That’s because it takes just two or three minutes to draw the solvent you need. That’s quite different from distillation, which requires you to set up, distill and purify an installation. Which takes forever, and also takes up much more space. Add to that the fact that a lot of students work here. They would need help and supervision in setting up a distilling station. Using the automatic purification system is much easier. You only need to show them once or twice and then they’re good to go. The main advantage, however, is that the system is more controllable and safer, because it releases no heat. The students feel comfortable using it, and don’t have to deal with ‘distillation stress’. The worst thing that can happen is that the solvent comes into contact with the air, which means it is no longer completely dry. But that hardly ever happens.” Changing filters The system has been in place for five years or so, Elferink says. “The only thing we need to do is periodically replace the filters. Our staff keeps an eye on whether the filters are still working, or whether we need to change them. Other than that, the system just does its thing – which is fortunate, because if it broke down we’d have a problem. It would delay our research, which would not make us happy!” On that note, can we expect breakthroughs in their sugar research any time soon? “Haha. Let’s see, how can I answer that without giving away anything confidential? Let’s just say there’s a dry paper in the works!”
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