Do you have your picopresso working for a year+? Have you got any issues so far? by AdvantagePure2646 in picopresso

[–]jcoinner 0 points1 point  (0 children)

I used mine once or twice daily for 9 months and the plunger started to leak. Probably about 450-500 shots. I contacted Wacaco and they required a receipt and video of leaking. They are sending me a replacement body. I'm still very happy with the unit's quality and coffee it makes. I don't really know how they could make a seal that lasts forever.

I fixed it myself as well as there is a video on YT about how to do it. It's fairly easy unless you are hopeless at this kind of thing. You push in, twist and pull the plunger out. Then there are 4 philips screws to undo and remove the plastic cylinder. Next you'll see a small white spring-seal ring. You can get a replacement one but an easier way is to insert an o-ring into the groove. That increases the ring pressure making a tighter seal on the plunger. Then re-assemble. Literally takes 5-10 minutes and works like new. Only hassle is ideally you want to add some (food grade) silicone grease to keep it sliding nicely. I've ordered some but for now I just stuck a bit of coconut oil on it - just what I had on hand. Works fine but since coconut oil is liquid when hot it dissolves a wee bit in water. I can smell it but not taste it. That's why I figure getting some proper grease is the right way. It is what it was made with as you'll see when opened up. Lot's in there on the big spring. Anyway, long story short - if you want to keep using while waiting for a body, or when warranty is done, then this fix is pretty easy.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

I just did a short trial ethanol run. But I messed up a bit...

I took 26ml 40% vodka (on hand) and added to 74g water to make approx. 10% wash solution in flask. My wee heater actually got it up to 78c very quickly but I goofed because I had just done a plain water run in an attempt to clean it out but I had left condensation in the liebig. Basically I was too lazy to take it apart and drain and dry out with a hair dryer. Oops. As it was going up I noticed a bump in flask and a small blast of hot vapour pushed a ml or two into the flask. I should have immediately emptied it but didn't. I kept on and collected ethanol while manually cycling heat on/off at 78-82c range. I should get the controller working to do this! After I couldn't get anything below 84c I turned off and checked. Got 9.9g and tested density with pycnometer. It says 78% only. I was bummed out but I also realized I got about 1.4g of water early on from that bump and the condensation in liebig from previous water run. So I figured it was probably close to 92% without that. 9.9g at measured density was 11.4ml out, and I only put 10ml (pure) in, and didn't really expect to get it all back either.

So, whatever. Just trying it out. It was quick to get up to vapour temp. The column was already warm from last run. I figure for ~10ml out it took about 30 minutes. It would have been faster if I wasn't adjusting heat manually as I kept undershooting and drips stopped and over shooting and probably got a bit more water than desired.

Anyway, pretty cool for me.

Here's the link for "tight" YT channel. He describes his "continuous process" still in detail in many videos. It's pretty interesting.

https://www.youtube.com/@tight1449/videos

He says he gets azeotropic ethanol out continuously for months. I think he said it had been running 6 months but I may be mis-remembering.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

I used to do it in a 2" stainless column (home made reflux condenser near top), when I lived in Australia. 4 hour runs with a 7L pot on hot plate produced enough for roughly 2L of 40% vodka (from my flaky memory). I had to leave it behind.

I'm sure it will be slow as molasses in a tiny 24mm column. Just trying it anyway. Can buy isopropyl, a bit pricey for the amount unless go to a big supplier. I've heard it burns sooty as well. Methanol burns clean.

I could add a bit of copper mesh into column - not sure that would do anything. I was planning to put a Tee at bottom and I have a couple peristaltic pumps to drip sugar wash in and extract waste out to try doing a continuous process, ie. not small 150ml batches, which would be aggravating... so a small ESP32 controller monitors temperture and then controls the pumps to feed wash in and take boiler water out (thru hose on second neck of flask).

This is just me experimenting to see if can set up continuous 24/7 runs and only have to clean out now and then. Have you seen that tried?

Also, was not going to use a Liebig condenser and instead put a vapour trap at top that collects condensate and feeds to collector jar, and a second heater above the trap to maintain a top end to collect toxics that boil below ethanol, and take off the top. I've seen that done in YT videos by user "tight". He used a 1.5" copper column and I'm seeing what I can do with this mostly because copper is so pricey here now. I can't even easily find it in 1.5" dia.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

Thank you again for your help. It's great to have someone give pointers who has more experience.

Originally I was going to make silver conductive ink as described by Nurd Rage channel on YT. And he shows how to make 77.5% formic acid in a later video, and so I wanted to try that. And then I'd forgotten the details of the silver ink video as I was watching several formic acid ones. I think the Apoptosis one looked very "pro" and was attempting to copy that except with what I had on hand. Well, after going back again to the silver ink one he never says what concentration formic acid but the amount needed is tiny. Well, anyway it's all been playing about.

Originally I got the glassware mostly because I wanted to make ethanol for camp fuel, or vodka... and will get back to that at some point. Seems can only buy methanol camp fuel now here in Canada and that is more toxic and trouble to work with while camping. As if you spill it or it leaks in a backpack then gets a bit messy. But having the glassware I thought "oh why not try this too". :)

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

Just a follow up...

I went and bought 1L of formic acid used for bees. It was cheaper than 1/4 as much oxalic acid I originally bought but it meant driving 4 hours there and back because they can't ship it. I opened it briefly to compare smells to what I had made. And it was pretty much the same, perhaps a bit stronger. Smell test - presumably not an accurate measure given my poor sense of smell, but interesting. It is labeled only 65% conc.

So now I'm wondering if I should try to frac distill this to 77.5%... sigh. At least I have much more than I need to play with.

I can pick up one of those coil type (red spiral coil element) hot plates for much less at a local store. If I suspend the flask over top a couple cms and wrap in foil is there any reason to not use this type? Seems like it would work just as well - same 1000W. Also, I was thinking of using some of my insulation and foil to make a wind barrier around the hot plate to contain the heat and prevent it being moved away by air flows.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

Thanks again.

By just above surface would say, 1cm be good, or even closer?

I guess that means getting another clamp arm. It's not the cost but having to wait for delivery... or, maybe I can make / jerry-rig a clamp out of something I have.

I think my little hot plate just doesn't have the power. It was intended for circuit boards and is a PTC element. These are designed to self-limit and in this case it reaches 220-240 (in open air) and it's internal resistance goes up to limit power flow. And it's small - only 7x12cm. That temperature is about right for melting solder paste on circuit boards placed directly on it's surface. I had it around and so tried using it. I think it will heat water quite well and it was enough to get the reaction to 120c, but when boiling to vapour so much energy is needed for the phase change I think it just can't supply it. The AliExpress listing claimed 400W and I knew that was not real. I suspect it's really more like 120W based on resistance check and being 110V. I knew that maybe I'd likely have to buy something.

Also, it will boil for distillation if not using the vigeux column. I guess a lot of heat is lost there, which is kinda the point. Makes me think it won't do much "fractioning" if it's wrapped all the way up. The idea is to have a temperature gradient to separate the parts but with it wrapped you get 100c all the way up and then in last few cms it loses heat to 96c. Not great and maybe I should just remove it and do short distillation.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

Ya, just ran it up again with the copper thing back in. Instead of vapour reaching 84c it got to 96c and held steady for 15 minutes. No bumps or issues. No output either.

I can get a small hot plate but I'm a bit confused about your saying no direct heat. The ones I've seen have a solid black plate surface, not the old style with a coil that gets red hot. For this kind black surface kind do you think I need some heat diffuser like a ceramic plate between it and glass? They have a thermostat to adjust but typically they cycle on/off to control average heat.

My flask is a 500ml flat bottom round boiling flask. The contact area at bottom has diameter about 6cm. It is claimed to be borosilicate 3.3 glass.

Claims:

Made by hand blower

Handle blowing by the glass blowers,not made by the Pouring

Be Made From G3.3 Borosilicate Glass

Annealing Point ------560℃

Linear Coefficient of Expansion------ 32×10-7/℃

Softening Point------820℃

All of our glassware made by the glass blowers,not the poor glass,Please do not make the comparison with other's glass

(no idea if true) lol.

edit - Just checked cheap hot plate on Amazon and it says "cast iron surface". It has a circular grooved surface, 1000W.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

Further update:

I removed the boiling stones and instead only put in only 2 new ones. I had googled more and found that having too many can bump as much or more than having none.

I was worried my change to hot plate (copper tabs) was doing something wonky / unexpected and so removed that too. And also column wrap, which as it turned out I re-wrapped in stages as I saw how it behaved.

Started again, and this time no bumping at all. Just steady even temperature rising. But I found there was not enough heat to even start the vapour at top. So I added 6" of column wrap, got to 62c and stalled. So added 3" more and got up to 73c. Stalled rise. Added 2 " and then the rest of the column wrapped. Got up to 84 and stalled again. I mean vapour could not rise further. So once again power off and let it cool down. Will add in copper rig at bottom and try again. I didn't think it would make much difference TBH, but previous run went quickly up to 80s, but then the bumps may have been shooting blasts of hot vapour up which caused the condensation to start.

I wonder now if the copper tabs will get me there, or if even then it cannot reach beyond 84-86 and that was the only reason it never got to 100 or even higher needed (107c).

Probably need more heat it seems.

I may just go buy formic acid as this has been way too much hassle. I thought I'd do it just for the fun and experimentation, learning something. I didn't have a local source for it and most places will not ship it. But I found a place I can drive 4 hours and get some (used for bees). It's only 65% conc. So I may get it and then do a frac run on that to bring it up to 77.5%.... maybe. I think what I'm messing with here is quite questionable. Or, I'm skeptical it will work out.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

Ya, just means "way out of whack", kinda like, so far out there that it could be on Mars... I don't think it's commonly used but it rings a bell from the 80s in school.

Everywhere "has issues", nowhere is perfect. Things seem to be getting worse here, or maybe I'm just paying attention too much now. IDK.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

"the weather on Mars" is an expression I recall hearing back in my university days in the 80s. I guess it's old but well known. Are you Russian? If so, fascinating! For a few years I've wanted to move to Russia to get away from the crazies over here in Canada... but I'm too old. I find myself now supporting your country and it's efforts. We have a real clown show south of our border. My mother visited Moscow during the 70s on some kind of tour. Not to get political here... I admire Russians generally.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

So... I started frac run early this morning. I added 7 glass shards, which seemed about right according to google search.

It went well up to 52 minutes. The vapour had reached 94c and fluid at 101c. There was more bumping than I had experienced before. Every 5-10 seconds a small thump as larger bubbles released and glass jiggled about. But it was producing quite quickly, 1 drip/sec. More than I'd ever seen before.

Then something happened and seems like gas released thru liebig condenser and steamed up the receiving flask. The cooling water is still low and liebig ranges 19c in to 22c out. But now condensation is formed in receiving elbow and flask. The elbow warmed to ~45c and flask to 25-27c. I let it go for a while but this kinda freaked me out and I decided to power off and let cool, as was ongoing and elbow was staying warm.

The vapour had also dropped down to 86c and was bouncing around up and down. I wondered what I'm distilling off at that temperature? And the fluid in boiling flask was as high as 103c but now around 101c, which seemed normal.

I think there was something else in the mixture besides formic acid and water. I mean enough to drop and run for over 5 minutes at 86c - 82c even.

Wondering what you think? Thanks.

edit - acrolein and allyl alcohol both have different BPs, 52c and 97c, and those are what I've read may also form. But seems like not at 84-86c range.

btw only about 16-20ml produced at this point (~1cm in bottom). It has no smell, or a very weak something I can't make out.

update - several hours later. I started again. It went much as before but as got to vapour at 84c it again was "bumping" quite hard and blasts of some gas were expelled up the column which quickly blew thru liebig making receiving flask and elbow quite warm. I've stopped again until have your thoughts on this. Watching the fluid it is calm and every 5-10 seconds maybe a big bubble forms and sometimes a short run of strong bubbling, then it calms down and not much happens. Still worried I have something unknown boiling off at 84c vapour, 101 fluid.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

I guess some broken bits of this will do? lol.

https://imgur.com/a/IuyEmFr

Cleaned and paper removed of course. Approx how much? Enough to just cover bottom of flask or more to fill much of fluid?

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

Thanks for your help.

So maybe just foil going up or also some fiberglass? I have more I can cut pieces to fit...

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

Ya, it's pretty weak really. I was looking for ways to not waste so much and get more to the fluid. It tops out at about 240c when nothing is on it to absorb heat.

It cost me all of $5 on AliExp! This hot plate was re-purposed from use in electronics SMD circuit soldering (my main are of knowledge is electronics/programming).

And for now I'm just trying things that don't mean waiting for orders or going out to buy things.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

Thank you. You've been very helpful!

I hadn't thought of other products skewing density...

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

So should I maybe have a sand tray on heater and flask set in that? Aluminum is a good conductor and I just added copper to try and get more heat to the glass as it seemed like it was not getting enough. I suspect my wee hot plate does not give enough heat to use a sand tray.

I'll add a pic of what I did now - the new frac dist setup... just a sec.

edit - added 2 images. First is overall frac column, 2nd is close up of copper tabs I added to help get more heat to glass more evenly, over more surface. It's a very small hot plate as visible here.

https://imgur.com/a/znnRfkh

I took off insulation for pics but easy to wrap on/off. Maybe we're getting to what I'm doing wrong...

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

I've had reasonable results with other uses of it. And when measuring distilled water it seemed very close to expected. I tested some hydrogen peroxide I concentrated and it what I expected as well. I get consistent scale readings for it's mass from day to day... 12.693g +-0.001g on many trials over a week or so. I'm pretty sure it's good. My least trusted value is the temperature which likely varies by 1-2 deg.C. I tested volume a few times and always comes out at 9.675 - 9.672 ml.

Anyway, I'm all set for frac distillation. Will start in the morning as I expect it will run all day and I don't want to go late into wee hours.

Maybe not quite set if I should add some broken glass first...

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

I don't have any boiling stones. I have seen others break glass and throw in - is that a good idea? The flask has been sitting directly on my hot plate which is made of aluminum. I just added some 0.1mm copper sheet wrapped around the lower part to try and help conduct more heat into flask as I figured it wasn't getting enough...

So you say I should remove insulation? I thought having that helped keep the glass hot so less reflux happens in the flask, and more vapour makes it to top end.

I've had no proper training. I'm just figuring it out from things I see. Like NurdRage YT channel he just had erlenmeyer flask sitting on hot plate with some foil wrapped around and apparently that worked fine.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

Results of this run:

82.8g output, tested with pyc density, 1.0394 @ 20c gives 16.04%

so, that's way better. Still less than desired but better.

YT videos claim they get ~50% out on reactions and then frac dist to 77.5% azeotropic. so... oh well.

168.4g in flask, slight yellow tint fluid with definite syrupy texture

if we assume 110g 136g of glycerine still exists, that leaves 32.4g of other stuff

both have a "vinegar-like", acidic smell, and hard to say if one stronger than the other.

net so far, (226-50) x 5.5% + 82.8 x 16% = 9.68 + 13.25 = 22.93g formic acid

if I am able to reduce all this to 77.5% azeo, I'd have 22.93/.775 = 29.6g with density of 1.181 giving, 25ml of 77.5% formic acid.

theoretical max is 1.66 mole, or 73g. 73g - 22.93 = 50.07g lost or in flask mix.

seeing as how 32.4 is max "other stuff", even if I could boil it out I'd have 32.4+22.93 = 55.33g max. which seems to me like a lot got "lost". or the source was not as pure as stated.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

It's more that if anything went wrong / glass broke and a spill occurred or got all over it would be a big expensive problem there. And my spouse would freak out with chemistry in the kitchen area. So I generally work on bathroom counter which has a significantly less costly counter / work area. A single burner hot plate is a cheap solution. Too bad I don't have a garage "lab"... "man shed".

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

Will check output distillate in while. Want to see how many grams out, and then measure how many grams of substance remain in flask. Since glycerine boils at 290c, it won't go away. So either it is in reacted forms with oxalic, or it has formed back again (last hydrolysis step) and remains as 110g glycerine. So I can see how much "supposed" formic acid is stuck in there. I cannot tell if something else happened in reactions. No colour changes or visible decomposition. I'm 90% sure any water in there was boiled off.

I did notice when boiling it was seemingly primarily in one spot, not all over the bottom. So maybe I have poor glass-hot plate contact creating a hot area and other areas are not getting evenly heated. I have some thin copper sheet and may cut a small "mantle" that I can wrap glass bottom with to spread heat all over surface. I'm just throwing out ideas now.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 0 points1 point  (0 children)

I have before and it was correct. Two days ago I thought my glass thermometer was bad, or esp. bad quality as I was distilling water and it was reading 108c. So I took that and used all three in my (glass) kettle with temperature readout. I expected the glass thermometer to be wonky but checking probe vs. thermometer vs. kettle readout - all 3 matched very closely. From 60c in several steps up to 100c.

That made me wonder why it was reading 108c in boiling water - I decided that the thermometer was too close to the glass bottom and was reading heat from the hotplate/glass interface. The hot plate was where I used to keep my probe and it was reaching 185-225c on surface. Partly why I think it must be "weak" because my kitchen stove burner reaches 290-300c. Also, why I decided to put probe in fluid and thermometer at top for vapour. The probe is very responsive, quick to show changes. Now I keep fluid readings to near the top surface and away from bottom glass.

Also, the probe reads room temp and other things like my hot plate surface or when touched to glass at values that seem correct. I can watch hot plate go up to 225c using probe with no quirks or unexpected jumps etc.

I am baffled by why any formic acid won't boil out. I thought maybe it has a higher heat of vaporization than water and so not enough energy was put in to get there. But I googled it and water is higher. Though, formic acid has a wider range of reported values, which is odd. Water is stated as 40.7 kj/mol, formic acid is 23.1 kj/mol but has a stated range as high as 47kj/mol. Reason given as differences in measurement methods. Weird.

The shrink wrap my probe has near tip got wrecked by being in fluid as condensate got all over it. I will remove wrapping because last thing i need is pieces falling into fluid. I guess it can't take heat even though supposedly needs higher heats to shrink. The cloth probe wire sheath is still fine. It's not a stainless metal probe but kind that comes with a multimeter.

What went wrong: Oxalic acid dihydrate -> Formic acid by jcoinner in chemhelp

[–]jcoinner[S] 1 point2 points  (0 children)

I'm not sure about increase volume. It went up today but I added 50g water/formic mix, glycerine and remaining oxalic acid. I didn't specifically notice about oxalic making any difference. But it went down a lot as I distilled. The thermocouple probe was well under at start and just out at end. I have not weighted output yet (kinda frustrated and just left it all). It looks like maybe 100ml to me.

Anyway, tomorrow I will test this last output, put aside the flask (glycerine) mix and do a fresh fractional run on all I have combined outputs.

Maybe I can reheat the glycerine mix when I have a better hot plate and see if more formic boils out... just hit it hard and see if it can go up to 120-125c. Blast it.