CalwiseSpirits

16 hours ago, Kindred Spirits said:

What type of carbon do you use? I know I have found some to be better than others for use with spirits. 

What proof are you filtering at?

I've used Geosorb and a carbon cartridge filter. I filter at 45-50% alc. 

What set up are you using for your carbon filtering? I'm trying to improve my carbon filtering protocol for my white rum and vodka. So far I've used two different methods:

1. a carbon fiber filter from TCW - it works, but doesn't remove as much flavor as I'd like. I think it works best for "light cleaning"

2. I mix a powder called Geosorb from Laffort into the spirit and wait a month for it to settle out. Then I filter it through several steps of cartridge filters all the way down to a .2 micron absolute filter to get all the carbon out. It's super time consuming and expensive and ruins my filters. 

Option #1 is easy but doesn't give me the results I want. Option #2 gives me the flavor results I want but isn't practical.

I want to be able to filter 1,000 gallons of spirit at a time. In my research it appears people are building their own carbon filters by filling a triclamp spool with granulated carbon and pumping the spirit through it.

I'm thinking of getting a 4"x48" spool, fitting it with #100 mesh gaskets, and filling it with 12x40 carbon like this. It sounds like with this set up I will still have to filter because there will be some dust that comes off of the granulated carbon but I imagine it won't be as bad as filtering out pure powder (with a cartridge filter? Would it be easier with a plate and frame or something else?)

Is this a good route to go? Would you recommend a different method? Are there any activated carbon suppliers that you recommend?

Thanks in advance for your advice!

On 6/29/2022 at 1:19 PM, adamOVD said:

Sounds infuriating. We were never contacted. Hopefully you are in the minority.

It's pretty annoying and flies in the face of the promise the FDA made to not go after distilleries who were doing their best to do the right thing.

Were you ever inspected or audited by the FDA for your hand sanitizer production?

I thought the FDA harassment saga was long over, but it reared its ugly head again last week.

In December of 2020, the FDA selected me for a random inspection, audit, and sampling of my finished product. I provided them with all of the batch documentation that they requested. I was told by the inspector that I would hear shortly if there is an issue after analysis of my products but that no news was good news. Months went by... I heard nothing... until last Friday.

18 months after my inspection, over 2 years after my last production batch, and regardless that I deregistered, delisted, and sold out of my product last year, I received an email from FDA stating that they detected unacceptable levels of impurities in my sanitizer and a whole laundry list of actions I need to take. I've heard of a few others who have also been receiving notices this month so keep an eye out.

This is absolute insanity. The compound they are alleging was found was acetaldehyde, which is a naturally occurring byproduct of fermentation and forms when alcohol is oxidized or in the presence of acetic acid. I only ever used USP-grade GNS or food-grade grape alcohol - I wasn't adulterating it or doing sketchy things like others were so I'm scratching my head over how it's even out of compliance.

The sanitizer we were making was meant for short term consumption to help out in an emergency. If they stuck it in a hot government warehouse for 18 months I don't think it's unfathomable that the composition changed as the alcohol slightly degraded. We're talking about parts per million levels here.

I'm trying to gauge how widespread this is:

Were you ever audited by the FDA?

Did you ever hear anything back - good or bad?

I did corrugated aluminum. Although it's a bit of a pain to clean, it cleans up nice. It's also hard to mount stuff to. But it looks great. 

I have had this issue. I tried to fix it with pectic enzyme and it didn't work. I suspect the high alcohol content denatured the enzymes. I think that next time adding the pectic enzyme to the fruit, allowing it to work, then adding the depectinized fruit to the alcohol would be the way to go but I haven't tried it yet. You can also give the bag filters at TCW equipment a try - I have had a good experience with them filtering out other high-solids spirits.

On 5/25/2021 at 10:52 AM, Silk City Distillers said:

Sulfuric acid is what’s typically used as a catalyst.  It needs to be a mineral acid.

22 hours ago, Foreshot said:

 

So to explain this a little (for everyone aside from SCD) - citric acid is a carboxylic acid where sulfuric isn't. Citric acid will take part in esterification reactions, sulfuric won't. So when you added Citric acid you changed what esters were being formed. If you used sulfuric it would have enhanced what esters were previously being made. You wouldn't change the flavor as much as enhance it. The flavor might change though as the catalyst will enhance all esterification reactions, not just the "good" ones.

Thank you for explaining that. It makes sense. I should have known.

Is sulfuric acid ok to use in distillation? Won't it decompose and form some nasty byproducts? 

On 5/20/2021 at 1:03 PM, Foreshot said:

The lower the ABV the more esters you're going to lose. Keep the ABV as high as possible for as long as possible. Water breaks esters apart. Acidity probably helps reform the esters. https://www.jove.com/science-education/11213/hydrolysis-of-an-ester

You also can have transesterification - it's where higher polarity molecules replace the acid side of the equation and it becomes a different ester. https://en.wikipedia.org/wiki/Transesterification

Thanks for the info. On Friday I actually tried an experiment related to this. I added a bit of dunder to a spirit run - great results, ended up with desirably funky distillate. On the next spirit run, I added dunder and citric acid. My theory was that citric acid would aid in Fischer esterification and magnify the flavors I achieved during the previous run. Nope. I found it destroyed the good esters I was trying to make and instead I got relatively neutral hearts and ended up with tails that tasted bitter and horrible. It tastes like some sort of salicylate (menthol/wintergreen) ester was formed as well.

On 5/22/2021 at 12:53 PM, Silk City Distillers said:

Noticed the same thing - unique ester profiles are seemingly obliterated after 1-2 years aging.  We really noticed this with our 100% rye - which had a very fruity profile at the 1 year mark, and nothing at all by the 2 year mark.  So much so, that regular customers actually asked us to bottle the younger rye.

One of these days I'm going to run a batch of rum, take no heads cut at all, and put it all into a barrel just to see what happens.

I second maintaining higher proof, barrel and bottle.

Yep, I've noticed it in my whiskey too. Isoamyl acetate (banana) in particular - which I don't necessarily want a ton of in my whiskey - but I want it in my rum and I can't get it to stick around!

I used to make very conservative cuts. Now if I'm making spirit that I plan on ageing, I'm going really deep into the tails. I'm starting to find going deep on the heads yields good results as well - as long as there isn't too much ethyl acetate.

interested

I've been experimenting with creating a super funky high-ester rum. However, I've been noticing that the esters degrade over time when it's barrel aged. I also made a Navy strength high ester rum and noticed that the esters degraded significantly after sitting in the bottle for a few months to the point where it was unrecognizable. Is there a way to stabilize the esters in finished spirit? My best guess is to add a little bit of acid (citric?) to the spirit but I'm not sure.

I've had this happen before too. My best guess is sulfur. 

2 minutes ago, Absinthe Pete said:

LOL No worries. I miss stuff all the time. Wish I could help. This stuff is useless to me too.

In my defense, I do know people who were purchasing organic GNS to make hand sanitizer because it was all they could find at the beginning of the pandemic. Crazy.

I'm still sitting on a few thousand bottles I'm trying to figure out what to do with. Better than 10 totes though!

14 minutes ago, Absinthe Pete said:

You're joking, right. It's denatured alcohol.

No, just blind... not sure how I missed that. Sorry. 

Is it organic by chance?

We make cocktail syrups at my distillery in addition to spirits. We've been using a 5 gallon brew kettle on an induction plate to heat our syrups and then bottle them through a small ball valve. We fill 8oz bottles and use plastisol-lined screw caps. I need a larger more robust set up, about 25 gallons. I'm thinking ideally we'd use an electric jacketed kettle with a small ball valve with a nozzle that can fill a bottle with a 28mm opening.

Does anyone else make syrups and have some equipment or production tips they can give me?

TIA!

4 minutes ago, Silk City Distillers said:

Try Greenfield Global/Pharmco.

https://www.pharmco.com

Thank you! Their prices are almost 2x of what I was paying at Ultrapure 😬

On a similar note, I'm looking for organic GNS. I usually get it from Ultrapure but they are having a hard time keeping it in stock. Any other recommendations?

13 minutes ago, Foreshot said:

Anyone have any idea how to deregister their location? I can deregister the Food Facility but no idea on the OTC part. 

This whole thing is so asinine...

My attorney contacted the FDA and this is the step-by-step email they sent:

1) The first thing you will want to do is delist the drug product. To do this:

1)               Login to the CDER Direct Account (https://direct.fda.gov)

2)               Click on “Product Listing and Reporting”

3)               Click on “Submission Accepted” for the most recently, previously submitted Product Listing

4)               Click on “Create New Version” (do not alter any of the information in the Header Details as it is correctly updated for you when you click “Create New Version”)

5)               Click on the edit tool (pencil/notepad) next to the Product NDC toward the bottom of the page

6)               Change the Marketing Status from “ACTIVE” to “COMPLETED”

7)               Enter an End Marketing Date that corresponds to the last lot expiration date

😎               Click on “Save Product”

9)               Click on “Submit SPL”

2) After that submission returns as “Submission Accepted” (takes about 15 minutes), then you may De-Register your establishment. To do this:

1)               Login to your CDER Direct Account

2)               Click on “Establishment Registration”

3)               Click on “Submission Accepted” for the most recently submitted Establishment Registration

4)               Click on “Create New Version” (do not alter any of the information in the Header Details as it is correctly updated for you when you click “Create New Version”)

5)               Change the Document Type to “Establishment De-Registration”

6)               Click on “Submit SPL”

When I was audited a few weeks ago my inspector told me that the FDA was considering implementing a fee, but I got impression that it was going to be on future batches, not retroactive. I did find it interesting that part of his report was the value of the sanitizer I manufactured as well as the value of my current inventory on hand.

If we are retroactively charged a facility fee, we need to create a substantial PR backlash. I'm already pissed off that they chose to audit us during the second wave of the pandemic. There were a lot of folk who didn't even bother registering with the FDA - they won't have to deal with an audit nor pay any fees. We're getting punished for doing the right thing. This is so egregious that part of me believes there's no way this is actually going to happen. 

beautiful piece

Glad (?) to hear others are having the same experience. Last week I received a call from an FDA inspector asking quite a few specific questions about my hand sanitizer production: how much did I make, what formula did I use, what packaging did I use, did I sell it out of state, etc. I politely answered his questions and asked him why he's contacting me - was there a complaint? He assured me there wasn't a complaint - they were randomly selecting distilleries to audit. He asked me to email him the records of my most recent batch (including the POs, BOLs, and COAs of the ingredients I used), sales invoices and BOLs, and labels. Fortunately I kept pretty good records of everything. He said he has been auditing a lot of distilleries but strangely he did not know what Bitrex is or what a TIB is. I also found it strange that he asked me for my labels considering I had already uploaded them to the FDA database when I registered. He asked if he could conduct a site visit the next day. I told him I was way too busy working to comply with a new state shutdown on my business and we scheduled a meeting the next week.

My inspection was today. It took half an hour. He just had me sign an affidavit stating that the documents I gave him were true, collected 5 bottles for samples, and left. I asked him if I would be hearing about the results of the audit/samples whether they're good or bad and he said that's a good question. 

I notice some of you were contacted September or earlier - did anyone hear back? How long did it take? Did you pass with flying colors or did they come back at you with errors in your paperwork or contaminants in your sample?

I agree with @Bob Morris and @Patio29Dadio's sentiment... knowing full well that distillers have no experience manufacturing medical drugs, the FDA granted us emergency authority to produce sanitizer during a time of dire need. Now that we're not needed anymore they're auditing us and expecting our records to be perfect? All while we're struggling to keep our businesses afloat during a second round of state-mandated business closures? The tone deafness is astounding. I understand the need to protect the public. There are some bad actors that need to be reprimanded. I would be more understanding if they were operating on a complaint-basis or taking random field samples but this random audit method right now is pretty burdensome. Many of us busted our asses to come to the rescue of our community and this is how we're being thanked. No good deed goes unpunished.

We generated a lot of goodwill in our communities. We have the public on our side. The few people I've told about this are appalled that the FDA would conduct themselves in this manner. I'm hoping it was just a relatively brief inconvenience and we won't hear from them again. But if they decide to go further I think it's important that we all band together and generate quite the PR backlash. Let's keep each other updated.

On 8/16/2020 at 6:42 PM, captnKB said:

@adamOVDI prefer to reduce proof in the barrel as the change in proof in the barrel will extract flavors out of the barrel that will not come out at a higher proof. Overall reduction of proof slowly in the barrel yields a softer more rounded spirit. Brandy makers in europe have known this for many years but the approach has not really been given much atttention in america 

I've been experimenting with this too. Not sure why this isn't common practice. 

Chill filtering may help

I'll make the same offer as @daveflintstoneand I'll even offer consulting services for $100/hr

Really interesting discussion. Thank you for starting this, OP, and thanks to all for bestowing your knowledge upon us. 

@Mountain Brewer I think this has already been made clear to you by others but for what it's worth I also think that you are making your cuts way too narrow. 500-600 gal of 18 brix mash yields me a barrel. Also, if you insist on using charcoal I would filter it through as fast as you can to minimize contact time. 

@JustAndy and @DrDistillation - what's the reasoning for distilling a stripping run below 20% abv? I usually stop my collection around 20-25% because I find that the cost of running the still longer considered with the yield isn't efficient and after that there isn't much flavor in it anymore anyway. In general, the deeper I go into the tails during a stripping run results in more tails and dirtier hearts on the finishing run. Overall my low wines end up being around 35%.