Sponsored Content: Lab Hacks

Lab Hacks

The tips for lab success that you won't find in a journal

By Mauro Mato & Rachel Brazil, C&EN Media Group Contributing Editors

Some of the most important knowledge in chemistry isn't codified in the literature: it's the tricks that get handed down from postdoc to graduate student to make laboratory work easier. "Lab hacks," as they are increasingly known, can be tools to make the lab run smoothly, tips for getting difficult equipment to work, or techniques for dealing with sensitive reagents. In some labs, hacks even extend to the ingenious repurposing of equipment to create Robinson Crusoe-esque solutions. Whatever they are, these lab hacks can make the difference between success and failure, and increasingly, chemists are sharing their hacks with their peers over social media.

We are more familiar with the term “hack” from the world of computing, where it refers to modifying or altering computer software. Today the term is used more widely to describe a do-it-yourself solution to any problem. There is even a website dedicated to IKEA hacks—clever modifications of IKEA furniture. Chemists, particularly in online discussion forums, have started using the term “lab hack” for tricks or strategies they use at the bench.

A tool for tracking inventory

Daniel Fitzpatrick, a Ph.D. student in synthetic chemist Steven Ley’s lab at the University of Cambridge, has managed to turn what started as a lab hack into a rapidly growing start-up. Finding their traditional lab inventory software was out of date and unable to meet their needs, Fitzpatrick and others in the group built their solution, tailored to the way they worked in the lab. They created a software package that would make lab management simple by tracking and organizing their chemical stock. The idea was to cut down the time group members spent searching for compounds in multiple labs.

“When things work well, you really do take them for granted, but these things can help increase your productivity,” says Fitzpatrick. His group designed a system that uses bar-code scanning for chemical identification and auditing and is cloud based, making it easy to share in one or multiple labs. Users can search for compounds using multiple names and structures on a laptop or even an iPhone.

The software was so useful that when people left the lab they still wanted to use it, Fitzpatrick says. “Ex-group members asked to use the tool in their new labs,” he says. “Word of mouth led to such demand that we set up a spinout company.”

That was back in 2014, and now ChemInventory software is used by more than 6,000 chemists in 74 countries. Colin Sambrook Smith, director of computational sciences and informatics at Sygnature Discovery, a contract research company based in Nottingham, England, is one of those users. His firm is using it for its 100-plus scientists: “Although it was designed for reagents, we are also using it for tracking pieces of handheld equipment in the chemistry lab,” Sambrook Smith says. “So we can track particular pieces of equipment where we’ve got just a few of them distributed around several laboratories.”

Lab Hack 101

• You were probably told this your first day in a chemistry lab, but it’s easy to forget how to do the washup. Multiple rinses using smaller amounts of solvents are better than only one with a large amount.

• Before washing an organic phase, remove aqueous residues remaining in the separatory funnel.

• If two pieces of glassware are stuck together by a ground glass joint, try heating them up with a burner or other heat source to separate.

• When using sticky chemicals such as iodine, use two pairs of gloves. When you are finished with the sticky reagent, take off the outer pair, and you are still gloved and ready to go.

Mind your product

Many of the hacks that chemists are communicating online in forums such as Reddit chemistry are the sort of tacit wisdom that has been shared and passed down in labs forever but is rarely formally transferred in writing.

For example, how do you weigh samples? Hacks recorded on Reddit include putting the whole reagent container on the balance, setting it to zero, and then removing the reagent until the balance reads the negative value of the amount you want. Need to weigh amounts below the accuracy limit of your balance? Weigh a larger amount, dissolve it in a known amount of your reaction solvent, and add the corresponding volume of the resulting solution. For tiny amounts of liquids, weigh the liquid container, zero the balance, and pipette out the exact amount you need, rinsing your pipette in solvent to make sure you don’t leave any behind. For weighing liquids with very low boiling points, chill them in the fridge or freezer first.

Pulling solvent from a precious new product is another area ripe for hacks. If you are having a hard time getting rid of those high solvent peaks to get clean nuclear magnetic resonance (NMR) spectra, Redditor Macabre suggests this trick: “Place the vessel in a dry ice bath under nitrogen or argon for 2-3 minutes, then bring it back to room temperature and apply high vacuum.” Doing this three times, Macabre says, will remove most solvents. Or after a column purification, redissolve the product in your NMR solvent before removing it under reduced pressure.

What can you do to recover your product that is stuck to the bottom of your flask after removing the solvent? “Many organic solids can be washed off the side of a flask with methanol,” says Redditor joca63. “Then you can filter and isolate a nice solid in a vial instead of having it stuck on the inside of a flask.”

Difficult reagents

Other common hacks involve dealing with difficult-to-handle reagents. Chemists on Reddit offer lots of well-worn tricks for using air-sensitive reagents. For example, to help keep air out between uses, use paraffin film or electrical tape to cover Aldrich Sure/Seal or similar reagent bottle caps. Also, use a 22-gauge needle that’s at least 6 inches long to remove reagents from such bottles.

When it comes to NMR spectroscopy of air-sensitive compounds, some labs have custom Schlenk line NMR adapters that allow an NMR tube to be filled with an air-sensitive compound in a dry deuterated solvent. But what if your lab doesn’t have one of those adapters? Try using a small rubber septum to stopper the NMR tube; it should have enough room to insert a needle from the Schlenk line to fill it with an inert gas and a needle outlet to purge the air and prevent overpressuring.

Using closed ampules of dried deuterated solvents stored in a glove box might be ideal for inert-atmosphere NMR, but what if this isn’t available? Redditors suggest passing the solvent through a plug of activated alumina—a pipette with a cotton plug will work. Adding some calcium hydride or potassium carbonate and then filtering it out is another way to dry the solvent.

Chemists on Reddit also offer tips on handling reactive chemicals such as palladium on carbon. Pd/C can ignite in contact with methanol, a common solvent for hydrogenations. To avoid that, completely cover the Pd/C with another solvent such as toluene, then add the substrate and the methanol. However, this approach could interfere with the experiment and cause unforeseen side reactions.

Saving time

Repetitive experiments are also ripe for lab hacks aimed at efficiency and maximal throughput. A good example is thin-layer chromatography (TLC). Have to run multiple TLC plates in the same solvent system at the same time? Try using a glass container filled with sand to hold up multiple TLC plates. Also, elute the spotted plate in a few millimeters of pure methanol. Methanol will concentrate the spots, ensuring neat separations.

Online lab-hack enthusiasts also have a lot to say about general lab management and how to optimize work practices. Fume hood management is a popular topic. Advice given includes leaving reflux condensers permanently connected and clamped in the back of the fume hood when not in use; just be sure to turn off the cooling water to avoid wasting water or flooding should a connection fail.

A washing bottle with its nozzle cut off is good to store and easily pours solids such as silica gel, drying agents, or sand. For solvents or reagents that you use on a regular basis, keep labeled test tubes against the walls of your fume hood containing a syringe and needles for use with each specific solvent or reagent. However, it is never recommended to use plastic material or reuse tools when you want to get clean spectra.

Ingenious hacks

Sometimes hacking requires chemists to look beyond the lab for inspiration. The ability to do this by thinking laterally and even by repurposing everyday objects is the sign of a true lab hacker. Fitzpatrick leveraged this kind of hack in a recent set of experiments he carried out to create a continuous-reaction process. Flow chemistry offers major advantages over batch methods, but it typically involves complex experimental setups. In 2015, the Ley group reported modular flow components coupled with control technologies to synthesize 2-aminoadamantane-2-carboxylic acid.

Fitzpatrick explains they faced a problem in achieving a continuous reaction, which included three chemistry and three workup steps. “In flow chemistry you pump and mix reagents through many tubes,” he says. “Tube diameters are quite narrow, so if you get precipitation in your reaction and formation of a solid, you may get tube blockage, which could lead to rupturing.” Fitzpatrick says they considered shaking the tubes in ultrasonic baths to make sure any solid produced did not stick to the tube walls. “But over a long period of time, ultrasound baths warm up, and it’s also a very expensive method.”

Instead, he and his colleagues came up with their hack. “We knew we needed a vibration device to stop the solids sticking, and we realized that all cell phones have a small buzzer in them that tells us when a text message comes in or a call happens,” says Fitzpatrick. So they bought some small motors that had balance weights on the end of them—the type used in cell phones. “We stuck that to the side of the tubing, one of them near the reactant mixing point. When we turned it on, the tubing was kept vibrating to an extent that the solids didn’t stick to the wall, so we solved the problem.”

Lab hacks are a big part of the art and science of chemistry. They help chemists get the best out of their instrumentation and be their most productive. But we often forget to pass this knowledge on. So the next time you come up with a creative hack, remember to share it with the rest of the lab—and the rest of us by using #labhack on Twitter or Instagram.