Why does your SPE disk need to be dry?

Every step within a solid phase extraction (SPE) procedure is imperative, but one of the most important steps that must be done properly is the air-dry step.  As you may know, the conditioning step prepares the SPE prior to the sample load to ensure that the sample load process will capture the analytes of interest within the media bed.  However, once the sample is done loading, there is a lot of water that is left on the disk.  Depending on the solvents that you are using following sample load and the analytes you are capturing, an improperly dried SPE disk could ruin your day.

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EPA Methods and the Use of Drying Techniques

Do you ever tire of using sodium sulfate to dry your extracts?  I know I do.  That is why, whenever I get the chance to avoid using it, I do.  The worst experience when using sodium sulfate is when you do not use enough of it, and the sodium sulfate reaches its maximum capacity leading to water breakthrough into your ‘what was supposed to be a dried extract.’  Then, you must dry the extract again with more sodium sulfate.  When you are a high throughput lab, redoing steps is not ideal.  Unfortunately, EPA Methods 525.2 and 525.3 require sodium sulfate drying as the drying technique, to name a couple, but not all EPA methods require sodium sulfate for drying.  That is why when there is an alternative technique available and you are permitted to use it, why not use it?!

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Improvements in Processing Drinking Water Samples by Method 525, Part 1 Sample Preservation

Since its release in 1995, EPA method 525.2 has been one of the most widely used methods for quantifying semi-volatile compounds in drinking water.  Chances are, if you work for or own a drinking water lab, you probably analyze for compounds in this method – at the very least, you’re probably at least familiar with the method.  This is a widely accepted method for quantifying semi-volatile organic compounds; however, there are some glaring issues with the method that the EPA has recognized and addressed.  These changes have been collected and implemented in a new revision – Method 525.3 – which was published in 2012.  Method 525.2 is still more frequently used by laboratories processing drinking water samples; however, I would argue that Method 525.3 is more scientifically sound.  In this 2-part blog series, I will address multiple aspects of Method 525.2 that have been modified to improve the collection, preservation, and processing of drinking water samples.  In this first part, I will focus on the improvements that have been made with respect to the sample preservation process.

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Solid Phase Extraction of Drinking Water – How do I Dry My Extracts?

If you’re a laboratory that’s processing drinking water samples using solid phase extraction, you’ve inevitably gotten to the step in your procedure where you’ve eluted your analytes from your SPE media and you find yourself saying “How do I dry my extracts?”

What’s the best way to dry my extracts? 

This is a question we get quite frequently and it’s a reasonable question to ask.  Unfortunately, the answer is – it depends.  Solvent drying (not to be confused with solvent evaporation) is an important step in your extraction process when you’re using organic solvents to elute your target analytes.  Residual water in your solvent can cause issues if your target analytes extract back out of the solvent and into the water while you’re trying to evaporate or analyze your sample.  Water can also damage your chromatography system, so if you’re quantifying your extracts by GC/MS or LC/MS, you want your solvent extracts to be dry prior to analysis.

So, given the importance in solvent drying, I thought I’d share some of the commonly asked questions that come up under this topic.

Q: I’m processing my samples against EPA Method 525.3.  Does it matter how I dry my extracts?

A: If your lab is being audited against EPA Method 525.3, you need to dry your extracts per the recommended procedure – in this case, sodium sulfate.  Make sure you purchase the recommended grade of anhydrous sulfate and store it appropriately.

If your lab processes a large volume of samples, you may have sought out alternative approaches to solvent drying, such as phase separation membrane.  While sodium sulfate is readily available for purchase in bulk quantities and is pretty easy to learn how to use, it has some potential downsides to it.

  • It has to be dried and carefully stored, which is time-consuming and requires you to have adequate drying and storage equipment
  • It has to be disposed of as hazardous waste
  • It’s a chemical that dries your solvent by reacting with water to form a hydrated salt, which means it can retain some of your target compounds (particularly those that are highly water soluble)
  • It can contaminate your extract, particularly if it’s stored incorrectly or purchased at a lower grade than is recommended
  • It can be saturated. What that means is, if you didn’t calculate the mass of sodium sulfate you needed, given the volume of water you needed to remove, you could exceed the capacity of the salt and end up with a solvent that’s not completely dry

Phase separation membranes physically separate the water from your solvent, which eliminates all of the challenges you face with a chemical drying agent such as sodium sulfate.  Plus, it’s compact and easy to store, intuitive to use and easy to dispose of.

There are a handful of benefits to using a phase separation membrane over sodium sulfate – just make sure you check the method you’re following and adhere to the drying method outlined there (if there is one).  Check out the method summary in this app note for an example protocol that adheres to EPA Method 525.3 guidelines.

Q: Since EPA Method 525.3 specifies that I use sodium sulfate, can I put sodium sulfate on top of phase separation membrane to dry my extracts?

A: While clever, this is an idea that you would want to run past your auditor first.  Since the method specifies the use of sodium sulfate but does not specify the physical separation of water (using a phase separation membrane, for example), physical separation isn’t forbidden, but it’s also not specifically allowed.  Yep, this one is a gray area so have a conversation with your auditor before cleverly devising a drying setup that includes both chemical and physical solvent drying.

Q: I’m running samples against EPA Method 525.2.  Do the same rules apply to me?

A:  Yes.  As with Method 525.3, this method specifies the use of sodium sulfate.

Q: I’m not processing samples against an EPA Regulated Method and my protocol doesn’t specify a protocol for extract drying.  What should I do?

A: If your lab is not reporting results against a method that specifies an extract drying method, you should have the option to decide whether you want to dry your extracts using physical or chemical separation (double check your laboratory’s established protocols to make sure your SOP allows you this flexibility).

If this decision were up to me, I’d order myself a huge stack of DryDisk® Disks and wave goodbye to sodium sulfate forever!

Do you prefer physical drying over chemical drying?  If so, let us know in the comments and share this post to spread the word!