A Deep Dive into NPP - Analysis/ Does the silicone tubing end up in the brew if you use a capsule filter filtration system?

[B Ware]

I recently received some unusual looking and smelling npp raws. This sparked my interest of going down the rabbit hole to analyze it. I haven't had a lot of time yet to dive deep into the GCMS of the unfiltered and filtered samples so I'm hoping to get your thoughts on them.






Below are the reports for the raw sample.











Once the unusual npp was brewed the unfiltered product had a lot of impurities floating around and you could not see through the beaker as it looked foggy. Quite frankly it looked dirty.




Unfiltered GCMS report











Below you will find the details of the finished filtered product. I decided to have it GCMS tested as well. I wanted to see if there was a difference in the reports after filtering all the impurities out of it. Most importantly I wanted to see if there were any traces of plastics or silicone in the final product that were not in the previous reports. I use a peristaltic pump, capsule filter and food grade silicone tubing and wanted to make sure the BB and BA were not dissolving the tubing and it ending up in the final product. I will note that it does look like my BA content seems severely off. I add 1.5% of BA to the brew but this sample shows quite a bit less than that.

 

[Photon]

I think the more important question is can silicone and plastics be accurately detected by GCMS.

Even when I completely dissolved plastic in BB and sent it in for GCMS, what showed up was something else instead, which was then used as a proxy for dissolved plastic. This leads me to believe only certain parts of what was dissolved actually showed up and many components remain undetected.

I don't believe GCMS is the right approach for testing for dissolved plastics, silicone and even syringe filters.

We're severaly limited in what we can test without using a large lab, spending alot more and breaking OPSEC.

The best we could do now is probably to search for spec sheets, seeing what material it's made out of, checking chemical compatibility tables..and to use solvent resistant equipment..

 

[janoshik]

GCMS is not quantitative, the % on the GCMS don't mean anything in particular, you can't compare it with relative concentration of BA ( 1.5% ) you added.

Cheers

 

[janoshik]

I think the more important question is can silicone and plastics be accurately detected by GCMS.

Even when I completely dissolved plastic in BB and sent it in for GCMS, what showed up was something else instead, which was then used as a proxy for dissolved plastic. This leads me to believe only certain parts of what was dissolved actually showed up and many components remain undetected.

I don't believe GCMS is the right approach for testing for dissolved plastics, silicone and even syringe filters.

We're severaly limited in what we can test without using a large lab, spending alot more and breaking OPSEC.

The best we could do now is probably to search for spec sheets, seeing what material it's made out of, checking chemical compatibility tables..and to use solvent resistant equipment..

Point to consider: Plastics burn, burning products can only be detected, not plastic itself.

 

[janoshik]

GCMS can only detect substances that are volatile, which is its major limitation.

 

[B Ware]

Thanks guys. I think we are all definitely seeing the limitations of GCMS.

 

[readalot]

Point to consider: Plastics burn, burning products can only be detected, not plastic itself.

Why was the siloxane peak dismissed when it only showed up on the filtered sample?

Was a blank run? How do you know if it came from the liner, column or the sample?

https://community.agilent.com/technical/gcms/m/files/602

Adding GPC or headspace GC to your arsenal of tools anytime soon?

Very curious change on the TICs going from raw to unfiltered samples.

 

[janoshik]

Because it depends on the state of the GCMS and the time we last cleaned it more than anything else.

No headspace in plans, but NMR can do some stuff it'd be used for.

 

[janoshik]

About GPC meaning gel permeation? We already do that.

 

[readalot]

About GPC meaning gel permeation?

Y

We already do that.

Thanks for the responses. Are you set up to quickly screen for soluble organic polymers (plastic), or are you referring to just your HGH SEC setup?

@Photon FYI, re: polystyrene.

 

[janoshik]

Y

Thanks for the responses. Are you set up to quickly screen for soluble organic polymers (plastic), or are you referring to just your HGH SEC setup?

@Photon FYI, re: polystyrene.

HGH SEC setup = GPC setup, the difference is not the setup but detector in the end.

We use fluorescence, which is AWESOME for big peptides/proteins, as they pretty much all fluorescence (and other stuff doesn't tend to randomly fluorescence with the same conditions).

However, plastics generally don't do that, so FL detector is impossible to use. They suck at absorbing uv too, but some do - but you'd need standards and the sensitivity is not great.

Refractive detectors are used, as they can detect *anything*. But they suck. They suck hard. They are the LEAST sensitive detector there is and it is outright impossible for them to detect low amount of contamination. They are used for testing raw plastic.

GCMS is so many orderds of magnitude more sensitive it's not even funny.

GPC is not the way here.

 

[gainslol]

@B Ware

Thanks for doing and posting this.

Just in case this helps, canola oil was found to separate microplastics from soil and fish tanks. It adheres to plastic, becomes kind of like a sediment, and then after that the recovery rates are pretty impressive (sometimes 100%). I would think the sediment won't make it past a filter.

But the next question to that would be, what to do with the canola steroids. There are some pharmaceutical injections that do have canola as carrier (I might have actually seen some homebrews with it). So maybe it could be used in small amounts and then mixed with the majority being MCT oil or something.

These are just some thoughts I had. There are a bunch of papers about it online. Here is a shorter one:

 

[readalot]

HGH SEC setup = GPC setup, the difference is not the setup but detector in the end.

We use fluorescence, which is AWESOME for big peptides/proteins, as they pretty much all fluorescence (and other stuff doesn't tend to randomly fluorescence with the same conditions).

However, plastics generally don't do that, so FL detector is impossible to use. They suck at absorbing uv too, but some do - but you'd need standards and the sensitivity is not great.

Refractive detectors are used, as they can detect *anything*. But they suck. They suck hard. They are the LEAST sensitive detector there is and it is outright impossible for them to detect low amount of contamination. They are used for testing raw plastic.

GCMS is so many orderds of magnitude more sensitive it's not even funny.

GPC is not the way here.

Thanks very much for the details and insight around what is at your disposal.

So what would you recommend? Find a lab with FTIR?

 

[janoshik]

Thanks very much for the details and insight around what is at your disposal.

So what would you recommend? Find a lab with FTIR?

FTIR is useless for <20% unknown components as well.

Pyro gcms or lcms but I can't imagine anyone be keen on doing that.

 

[readalot]

FTIR is useless for <20% unknown components as well.

Pyro gcms or lcms but I can't imagine anyone be keen on doing that.

Now you have me curious. Surely there are non destructive methods available for trace soluble polymers. Appreciate your response.

 

[janoshik]

Now you have me curious. Surely there are non destructive methods available for trace soluble polymers. Appreciate your response.

Shrug. Not my specialisation.

 

[readalot]

Shrug. Not my specialisation.

Would be some elbow grease.

https://4spepublications.onlinelibrary.wiley.com/doi/10.1002/vnl.22188

Maybe pick up some PS oliogomers plus additives. LOD a concern as you rightly stated.

A bunch more papers with MPs, NPs, extraction and analysis.