MFH - Experiments & Materials

[mesOUD]

Messed up concentrating an Erica tincture. Fell asleep and woke up to dried powder sticking to the entire inner surface of the vacuumchamber. Anything volatile long gone into the Dutch sky.

On a bright note, cleaning up the mess got me properly awake again😒

2-3 years ago İ have lost 1 distillation like this
Almost same

 

[MaxFromHolland]

2-3 years ago İ have lost 1 distillation like this
Almost same

Auch!

 

[MaxFromHolland]

White pine needle extract
Left per my normal MO, right is a macerate of the 'concrete' in jojoba. Smells like forest in the heat of summer, very dry.

Cambodi inspired* 'attar'
#1 I tried to get an animalistic opening note, red florals, honey and wood
(agarwood incense powder extr, propolis extr, red champaca abs, valerian extr)
#2 red florals straight away, slightly boozy honey and wood
(agarwood incense powder extr, propolis 'concrete' macerate in amyris, red champaca abs)

*Not similar smell but similar combination of notes

 

[MaxFromHolland]

Messed up concentrating an Erica tincture. Fell asleep and woke up to dried powder sticking to the entire inner surface of the vacuumchamber. Anything volatile long gone into the Dutch sky.

On a bright note, cleaning up the mess got me properly awake again😒

What could be recovered as dry powder i did put in a bit of oil and just tried some. From the bottle it smells sour-floral if that makes any sense. In the drydown though, it becomes quickly a kind of minty/camphorous toothpaste scent against a weak floral background.
I'll do a new batch at some point, will be interesting to compare.

 

[MaxFromHolland]

Was staring at some leftovers from previous failures:

Vacuum chamber with Acrylic lid - bought without knowing that the lid cannot withstand alcohol vapors (started to see micro cracks on the inside), now replaced by one with a glass lid

Heating mantle to create sort of a vacuum oven, which -duh, ofcourse- doesn't work because in a vacuum there's nothing to transport the heat from the wall to the liquid

Then it occured to me that i was only one cheapo ($2) fermentation lock away from creating a nice temperature controlled fermentation vessel:

Better than to have all sorts laying around unused🙂 Lid is heavy enough to keep a decent seal and else i find something to weight it down. Between vessel and floor there's a insulation layer with was also leftover from the vacuum oven fail.

 

[MaxFromHolland]

Strawberry plant (leaves+stems) extract turns out to be quite funky/ cheesy. Perhaps in combination with ambrette extract useful to create musk accord, for example. I dont know..

 

[MaxFromHolland]

Figured that instead of putting a bowl in the vacuum chamber, i might just as well use a borosilicate bowl as chamber.
Size and shape are ok to retrieve the concentrate and it save me the constant worry about bumping and splashing, or so i think.
Testrun time 🙂

Edit: this turned out not to be safe! After doing some math, the rim seems way to thin to handle the force applied due to the vacuum. The bowl handled it just fine, but without decent safety margin it's asking for trouble.

 

[Mr.P]

Figured that instead of putting a bowl in the vacuum chamber, i might just as well use a (borosilicate*) bowl as chamber.
Size and shape are ok to retrieve the concentrate and it save me the constant worry about bumping and splashing, or so i think.
Testrun time 🙂

*Pyrex food bowl
View attachment 54011

Wait, you're pulling a vacuum on that glass bowl? That sounds extremely hazardous to me. Unless it's a very low degree of vacuum.

 

[MaxFromHolland]

Wait, you're pulling a vacuum on that glass bowl? That sounds extremely hazardous to me. Unless it's a very low degree of vacuum.

It's sitting outside during the testrun for a reason... But its 4-5mm borosilicate glass and dome shaped so it should be fine.

 

[Mr.P]

It's sitting outside during the testrun for a reason... But its 4-5mm borosilicate glass and dome shaped so it should be fine.

very good! I know with scientific glassware some is rated for vacuum and some isn't (I was looking at glass desiccation chambers at one point) and if you're confident it's safe and taking precautions just in case, that's great.

 

[MaxFromHolland]

very good! I know with scientific glassware some is rated for vacuum and some isn't (I was looking at glass desiccation chambers at one point) and if you're confident it's safe and taking precautions just in case, that's great.

Your concerns are appreciated and I added a warning to the original post, better safe than sorry after all👍

 

[MaxFromHolland]

Figured that instead of putting a bowl in the vacuum chamber, i might just as well use a borosilicate bowl as chamber.
Size and shape are ok to retrieve the concentrate and it save me the constant worry about bumping and splashing, or so i think.
Testrun time 🙂

Edit: this is 4-5mm thick borosillicate glass. Do not try pulling this off with some random salade bowl or even with boro if it's scratched or otherwise damaged!

View attachment 54011

Hmm
Applying some math to check,
I put a force of more than 1000 kgs on the glass in the above setup. The rim of the bowl should be around 1cm or better as that is the weak spot. So this is indeed as @Mr.P warned way to risky!

Pitty because it seemed to solve an issue.

 

[MaxFromHolland]

Still had this jar of beetroot tincture with a lot of water from insufficiently dried beets mixed with the ethanol.
After filtering i put the liquid in the vacuum chamber for quite long while stirring, to pull the alcohol out.
Which left me with the water part. I added jojoba and put it on a stirrer for 24 hrs. Then left it to settle a few hours and put it in the fridge.
I just removed the solidified jojoba from the jar, dabbed the pieces with kitchen towel to remove water attached.
Now scooped into a funnel to melt and drip into the bottle:

 

[MaxFromHolland]

Strawberry plant (leaves+stems) extract turns out to be quite funky/ cheesy. Perhaps in combination with ambrette extract useful to create musk accord, for example. I dont know..

Just tried some on my skin. Really an interesting musky scent. My extract is just a bit weak. I converted 100g of dry matter into 10ml oil. 250-500g is probably better, maybe infuse some alcohol with multiple batches. Guess a soxhlet would be useful for this one.

 

[MaxFromHolland]

Still had this jar of beetroot tincture with a lot of water from insufficiently dried beets mixed with the ethanol.
After filtering i put the liquid in the vacuum chamber for quite long while stirring, to pull the alcohol out.
Which left me with the water part. I added jojoba and put it on a stirrer for 24 hrs. Then left it to settle a few hours and put it in the fridge.
I just removed the solidified jojoba from the jar, dabbed the pieces with kitchen towel to remove water attached.
Now scooped into a funnel to melt and drip into the bottle:
View attachment 54030
View attachment 54031

Needs to settle a bit but first impression is a mild earth scent, like when you dig up some veggies and bring them to the kitchen.
Its one of the first tinctures i made 6+ months ago, hoping for some geosmine scent. (The geosmine i have makes me think of beetroots so i thought maybe its reversible 🙂)

 

[MaxFromHolland]

Feel like rambling* a bit about why i tried that glass bowl as vacuumchamber 🙂

For me, extraction is a two-step process: reduction and finishing.
In the first step i take the 100-500ml of tincture and reduce/ concentrate it to 10-50ml. For this i like to pour the liquid straight into the vacuumchamber. Due to the evaporation, the alcohol cools down a lot and you need to compensate it by applying heat. This is much easier if the liquid sits directly in the steel chamber that sits on a 30-40°c hotplate, plus i get a nice large surface area. If i put the liquid in a bowl, the heat transfer is much less efficient which slows things down. This all is just fine as the, still liquid, concentrate can be easily poured out, and the steel chamber is easy to clean.
In step 2 i infuse a carrier oil with the alcohol and then remove the remaining alcohol. The result is 10-20ml of oil plus the solids that were dissolved in the alcohol. Usually a viscous/ sticky mixture. For this step i cant just pour it in the steel chamber for i wont be able to get it out without significant losses. So it has to sit in a smaller bowl where it becomes more viscous and cold as the alcohol evaporates, resulting in losses due to splashing no matter how careful i regulate the vacuum.
And there we are at an unsuccesful attempt to replace the steel chamber with a glass bowl, thinking i could do step 2 the same way as step 1 for the shape would allow me to recover the concentrate without losing so much.

Reset🙂
I don't have much trouble to remove the finished product from a small bowl, so maybe i should do step2 in a much smaller chamber? There seem to be various options like vacuum grade bottles** and flasks that have a stopper or lid with a needle valve and hose connector. Those can sit in a water bath to efficiently keep the evaporation going. Theres even a cute little mini version*** of my current chamber. (and even if i chose to put that 12,5cm lid on a small borosilicate bowl it would not be as dangerous for the force/wall thickness ratio is then at the right side of the safety margin)

Will have to figure out what is most versatile/ cheap. Would be nice to get that step 2 figured out properly so i can focus on the botanicals instead of the technicals..

* Told ya🙂
** https://amzn.eu/d/08IbdVDL
*** https://amzn.eu/d/06ARq1ya
(Links as example)

 

[MaxFromHolland]

Woke up with the birds
to get started. Dutch cherry wood, Vietnamese agarwood powder and a handfull of cherries, fermented for 5 days.

And no, I don't know what i will end up with. Time will tell (multi-day run)..

 

[Mr.P]

Woke up with the birds
View attachment 54058to get started. Dutch cherry wood, Vietnamese agarwood powder and a handfull of cherries, fermented for 5 days.
View attachment 54057
And no, I don't know what i will end up with. Time will tell (multi-day run)..

very interesting, I hope you come up with something excellent!

 

[MaxFromHolland]

Some fresh tinctures
Elecampane roots - floral
Birch (white) leaves - fresh spicy
Erica (Calluna vulg,) buds - musky floral
Catuaba bark - earth woody

 

[MaxFromHolland]

Feel like rambling* a bit about why i tried that glass bowl as vacuumchamber 🙂

For me, extraction is a two-step process: reduction and finishing.
In the first step i take the 100-500ml of tincture and reduce/ concentrate it to 10-50ml. For this i like to pour the liquid straight into the vacuumchamber. Due to the evaporation, the alcohol cools down a lot and you need to compensate it by applying heat. This is much easier if the liquid sits directly in the steel chamber that sits on a 30-40°c hotplate, plus i get a nice large surface area. If i put the liquid in a bowl, the heat transfer is much less efficient which slows things down. This all is just fine as the, still liquid, concentrate can be easily poured out, and the steel chamber is easy to clean.
In step 2 i infuse a carrier oil with the alcohol and then remove the remaining alcohol. The result is 10-20ml of oil plus the solids that were dissolved in the alcohol. Usually a viscous/ sticky mixture. For this step i cant just pour it in the steel chamber for i wont be able to get it out without significant losses. So it has to sit in a smaller bowl where it becomes more viscous and cold as the alcohol evaporates, resulting in losses due to splashing no matter how careful i regulate the vacuum.
And there we are at an unsuccesful attempt to replace the steel chamber with a glass bowl, thinking i could do step 2 the same way as step 1 for the shape would allow me to recover the concentrate without losing so much.

Reset🙂
I don't have much trouble to remove the finished product from a small bowl, so maybe i should do step2 in a much smaller chamber? There seem to be various options like vacuum grade bottles** and flasks that have a stopper or lid with a needle valve and hose connector. Those can sit in a water bath to efficiently keep the evaporation going. Theres even a cute little mini version*** of my current chamber. (and even if i chose to put that 12,5cm lid on a small borosilicate bowl it would not be as dangerous for the force/wall thickness ratio is then at the right side of the safety margin)

Will have to figure out what is most versatile/ cheap. Would be nice to get that step 2 figured out properly so i can focus on the botanicals instead of the technicals..

* Told ya🙂
** https://amzn.eu/d/08IbdVDL
*** https://amzn.eu/d/06ARq1ya
(Links as example)

Getting the puppy was a smart move. Finished this concentrate in roughly 1,5hr - cleaning included. More important though, with near-zero loss.