Lab Notes - August 31st - Nitric Acid from Calcium Nitrate and My Hotplate Failed, Again.
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- Опубліковано 4 лип 2024
- Some lab notes for the month of august 2020
I was exploring more nitric acid and wanted to see if calcium nitrate and sodium bisulfate would be viable. The rationale is that the reaction of calcium nitrate and sulfuric acid is well-known but almost never done directly since it produces insoluble calcium sulphate that solidifies into a rock in the flask. It has to be drilled out and risks break the flask. The traditional way to use calcium nitrate is the "wet process" where we first mix it with water and then add sulfuric acid. The calcium sulfate precipitates out and the dilute nitric acid is filtered and purified by distillation. This is slow and laborious so i was wondering if sodium bisulfate could be advantageous in producing a residue that didn't need to be drilled. This would save time and less risk of breaking glassware.
So i mixed 49g of calcium ammonium nitrate decahydrate with 150g of sodium bisulfate monohydrate and heated it directly in the "dry process" of making nitric acid. Nitric acid was distilled over and the yield was 85%. But more importantly the solid residue of sodium sulfate, sodium bisulfate and calcium sulfate was soluble. Upon addition of water it dissolved into a slurry that could easily be poured out. So i think the process is superior to using sulfuric acid as there is overall less labor involved.
For thoroughness i also tried the wet process by first dissolving the calcium nitrate in 50mL of water and adding sodium bisulfate. After distillation the yield was 95% but with 50mL of extra water diluting it. Personally i prefer higher concentration acid and don't mind the lower yields of the dry process.
Anyway. I was going to do additional nitric acid experiments but my hotplate failed.
Turns out the temperature sensor failed open and the safety limit of the hotplate refused to turn it on. It was a simple matter of finding the broken sensor and replacing it. The interesting note is that the hotplate uses a PT1000 RTD and it seemed the original was spot welded in. I didn't have spot welding capability so i used copper foil to crimp the connection.
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Came for the chemistry, stayed for the electronics debugging. Always a pleasant surprise when it's something simple to repair.
0:59 When I was a very young kid of only a few years old I got into the shed and tried to climb up onto the work bench. In doing so, I knocked over a bag or box of plaster of Paris and it fell right into my face and all over my body. It got right into my eyes and started rehydrating via my tears and my parents had to rush me to the ER. I don't remember anything other than being strapped tight in a straight jacket, hysterically losing my mind, as a nurse used a bag of saline and an IV tube to flush the plaster out of my eyes. :( My parents were traumatized. I'm lucky to have normal eyesight today. The shed remained locked at all times following that incident and I was officially deemed "a climber" and things were never kept on the countertops again. 😸 I hadn't done anything like that before, which was why I caught everyone off guard. Ok, thanks for stopping by to share this random traumatic memory with me. I have many more but they aren't relevant to plaster. 😇
reminds me of my father's story of almost getting eyesight damage from touching his eyes with sodium hydroxide-dirty hands
Our elders were tought
This is so random, yet has such a wholesome end to it. Glad you're OK, Mr.climber.
:)
@@fstech987 Thank you. :)
I'll admit I hadn't considered the possibility of a reaction leaving a Plaster-of-Paris casting in the bottom of the flask as a precipitate.
Just buy terminated sensors. They already have wire leads coming off them. I've seen them for 4 wire pt100 rtd sensors, so I'm sure they've got them for 2 wire pt1000 variants.
You can try discharging capacitor to spot weld PT1000s. You will just have to make a several trials to see what kind of energy is needed to spot weld the wires, and then just charge some large caps to get it to enough energy (and hopefully not to vaporize a sensor). After initial runs, it behaves quite/ consistently afterwards. This copper foil connection will oxidize and it can start varying a temperature, making a mess of experiments. Good news is they are failing safely (increasing resistance equals increase in temperature) but lack of heat can be an issue...
or he can use an epoxy www.jbweld.com/product/j-b-extremeheat to stabilize the connection But IMHO the sensor only needs be in the hole it doesn't need the leads so close to the hot plate... I would probably use a method that is not so permanent for the next time it goes out on you.
You can find a video on youtube for a DIY Battery Spot Welder. Basically just a car battery shorted to weld some tabs onto li-ion cells.
I think thats gonna be a relatively expensive capacitor.
@@htomerif you can tie a bunch of them in parallel also. I used to do that with some large 25 volt caps. Had about 6 of them tied together, used a bench power supply to charge them, and could spot weld pennies together. Touch one penny to the other and Bang! welded. For smaller things I would have to only use a couple of them or it would blast the lead right of a resistor or something instead of gently welding it.
@DinkleDigeroo Car battery is way more dangerous. Capacitors may be charged to non lethal voltages, but if capactances are sufficient, energy can be quite intensive to melt zinc - copper alloy from which leads are made!
I also prefer it when the broken part is relatively easy to replace, like a heat bed thermistor
Easy to replace, including the cost. Availability isn't the only key. And lobbyists especially want you to forget that. They'd rather you replace THE ENTIRE THING for AN ENTIRE LARGE PRICE. This modularity, however, is only possible when people work together to standardize things and modularize things.
Did you try power-cycling it?
I've always fixed all my own stuff. I love opening a circuit board and seeing all the chips. I collect transistors and capacitors amongst other things. I've recently started playing Minecraft again and falling in love with it. You can make virtual circuit boards that actually work using red-stone. Its all just logic and timing.
You can spot weld with 3 9V batteries and a couple of copper nails. It's not a long-lasting spot welder but if you need a one use unit it works really well. I needed one to connect the wiring to a copper coil induction heater. Same problem any solder would just melt.
Sweet that you managed to mcguiver the heatplate ^^
Never mind this request, just saw that it's just a disproportion reaction shifting KClO3 to KClO4 and KCl and then just recovering the KClO4 in acetone leaving the rest behind they are not soluble in acetone.
I am glad you are still making vids you have been very helpful in my learning
It's good to have you back...
Brazing is suitable for temperatures intermediate of soldering and welding.
brazing will burn most of the isolation away... because the temperature exceeds the temperature of the isolation... isolation can withstand 450°C...brazing starts at 600°C not considering the flame torch with 1600°C
This reminds me of a video by Cody'sLab from a couple of years ago (Nitric Acid From Thin Air) where he makes nitric acid using an electric arc. Probably not nearly commercially viable (certainly didn't seem like it with the setup he used) but a very low tech method if you don't have access to chemicals for some reason.
It's not concentrated acid, but I figured out that I could react the acid with sodium hydroxide to make sodium nitrate, and then react that with bisulfate, so it's good if you can't find potassium, or sodium nitrate.
Make your own hotplate already. Plate it, etch it, do some improvement to it. You got the power!
the previous hot plate videos were years ago? it feels like it was just a few months.
If your copper foil fails, try getting some small ID copper tubing (check the K&S metals display at your hardware store or order online) and crimping with a crimper designed for terminating PCB pin header connectors. I've used this successfully to terminate wires to fine nichrome resistance wire which is almost impossible to solder to.
i've soldered to nichrome wires but the bastard thing shrinks and expands too much and the join eventually fails. Your only real choice is lineman splice with lots and lots of contact surface.
Hello Doc.
Thanks for all
Thank you so much NR
THANK YOU ! This is a tremendous amount of help. I can throw an idea on low voltage/amperage welding of items. GTAW (Gas Tungsten Arc Welding) on a nearly microscopic basis can be done with Laboratory DC power supply or as I discovered when I was a young adult (adolescent), a 9 volt DC, couple of wire clip on leads, a piece of 3/32" Tungsten broken into 2 halves, some dry ice in a deep baking pan, low power welding lens, and a very steady hand. Have fun with that one, it is very pleasing accomplishment when done.
Nice I'd say you could make a hotplate repair playlist with the videos you have.
That's great that the calcium sulfate did not solidify and get stuck with the hot reaction.
Also, you can use the sulfates to act as a source of minerals and sulfur for garden plants.
Quite neat repair :)
I greatly look forward to the modernized nitric acid guide. It's useful for amateur chemists all around the world and (as you point out) could use an update/modern video.
Waited for this !
can you show the process of making nitric acid with oxalic acid and calcium nitrate? I haven't seen any youtube video's on it and I have heard lots of good stories about its concentration from just mixing the 2 chemicals in the right way. spoiler alert its something around 40% if you use near-boiling saturated solutions of both.
Looking forward to that nitric acid video!
Showing how you fix a problem sometimes is even better than showing the successful trials :)
Fan of your channel.
Great vid!!
Very nice video! This had topics I am very interested in.
Glad it was an easy fix! That said if there was a problem with the PCB I suspect it would have been not that hard to fix unless somehow corrosion got all over the board.
YES NEW NURDRAGE!
It looks delicious!
You might want to look into getting silver solder for those leads mate. It's used for jewellery-making, and it melts at like 600C.
Calcium nitrate is great source of nitric acid by the other way- if heated it generates nitrogen oxides (mostly NO2). No acids, no labglass, just heating in metal container with further absorption in water. I got also liquid NO2/N2O4 by cooling gases into NaCl/ice mix by this way.
But i'm not sure about stability of calcium nitrate in high temperatures. Is it safe to heating the compound up to 600 degrees C or more ?
Try using much tougher Triac, like about 30 Amps at 400 Volts or equivalent, that way the stir plate's heater will keep functioning for a good while. And heatsink it too.
As for the thermistor, higher temperature version with the same resistance may be more appropriate because the epoxy tend to dissolve in heat, messing up the thermistors themselves.
You might have problems with the copper foils, each heating will cause them to expand. Then they change position slightly, and eventually they will lose the electrical contact. Since you do not have the ability to weld, you need to crimp the connectors. The most available are probably the smallest ones car mechanics use or bootlace ferrules. Just strip the plastic off if any.
Is there any possible use for the residual products in the dry method?
Very true about the copper foil. I guess i'll just have to cross that bridge when i get there. I might see if i can electrochemically bond the connections if it gets really bad. That might be an interesting video it itself!
As for the residues. I'm not really sure. I suppose if you filter it, you can get crude calcium sulfate powder. If you heat it up to dehydrate it you can make your own plaster powder. Also calcium sulfate powder can be used as a catalyst support (but i'm not sure if i'll get that far on my channel). If you mix it sodium carbonate solution and stir for a few days you can convert it to calcium carbonate which is useful as a base for other reactions. Personally though, for the amount of work and cost, it might be more straightforward just to buy those end products. But i'll see if there is enough interest to attempt a recycling effort.
@@NurdRage glues like jbweld would work however i am thinking it would be best not to get the jb weld on the mica plates themselves.
@@NurdRage Electroplating the connection makes a lot of sense if crimping isn't good enough. But a good crimped connection can be good enough for aerospace grade parts so it will probably never come to that.
NurdRage out of curiosity, why the vocabulator?
@@Lossanaght Exactly. Crimping is the way to go.
You could also use some torch to weld sensor leads to wires (at least to several threads inside the wire) or just twist leads with wires tightly. Another way to weld thin wires is by using graphite rod (one from cheap zinc-manganese batteries will do) and some suitable power source. If IRC regular 120 VAC mains might work.
Ooh.. calcium nitrate isn't too hard to get..
The one I'd love to see is nitric acid from urea.. That I can still get by the bag.
That was a great video and of course you could fix them resistor sensors you're smart enough to do just about any damn thing that I've seen I wish I could do half the stuff you could course I wish I had more money than I might be able to anyways great video thanks for sharing
You sound different. Hope you’re ok :)
Please make a synthesis of dibenzazepine carbonyl chloride!! Eagerly waiting 🙏
Try finding robotics or electronics clubs in your local unis, they often have spot welders, or amateurs that like electronics
You might try an all metal butt splice. It should create a near permanent connection and be robust enough to not be jarred loose.
i'm glad these hotplates are easy to fix. Can you imagine if they weren't?
It would be nice if you could cover the electrolysis of KCl to KClO4 using swimming pool chlorination cells that use Rb,Ir on Ti anodes. Just wondering if they would hold.
easier to just thermally decompose imo
If the copper foil shorts out, won't the hot plate reach dangerous temperatures?
Wow! Another video in less than month! Maybe you could try to do some live chemistry on your channel, or twitch, or something?
I'm not sure how exciting it would be to watch a 30 hour reflux, but it's also true that it takes all kinds!
@@bielanski2493 i meant reactrions kinda simple but it would be still pretty nice, I think
@@piotrkrawczyk2390 chemistry is best done slowly. Chemistry done fast... is an explosion.
@@bielanski2493 isn't that what we all love?
@@piotrkrawczyk2390 yes, that's why I watch Hydraulic Press Channel!! :D
Nice fix on the hotplate. At this point, that thing is like a character on the show. It would be sad if you needed to replace it outright.
Use thin copper wire and tie knots to hold the sensor pins and their wires together.
@nurdrage I have a Corning analog heated stirplate you can have. Message me and I will ship it.
I convert my calcium nitrate to the more desired nitrates (eg sodium nitrate by using soda ash). This forms sodium nitrate and Calcium Carbonate at pH~7 which is highly insoluble, easy to filter, not as voluminous as calcium sulfate, and useful for neutralizing other metal (iron, nickle, copper, etc) nitrate solutions to scavenge the nitrate ion as calcium nitrate again to repeat the process. Of course, once neutralized the excess water will need to be removed to concentrate the nitrate in solution for the highest strength nitric acid when using the wet processes. Doing it this way allows us to use the Ca++ ion as a nitrate source and scavenger for recycling metal nitrate solutions. I can buy Calcium nitrate plus soda ash cheaper than sodium nitrate excluding my labor costs of course.
ya i did at first too but its easier to just use cano3 with nahso4 and boil with a small amount of hcl afterwards gets caso4 out real easy
What was the strength of the nitric acid from the dry method? Do you think could be a viable and economical means of producing higher quantities of 85%+ acid if you oven dry the chemicals beforehand relative to the 98% sulfuric acid/potassium nitrate method? The dry method looks as if you could VERY easily scale the process up to 2 - 4 times the size shown with relative ease and not have any of the potential dangers of large quantities of hot sulfuric acid.
Yeah it scales up no problem, it works even better large scale because it's easier to control the dreaded foaming.. i use 500g of kno3 and 850- 900g of sodium bisulfate in a 5 litre round bottom flask.. if you do it like this it's well worth catching the no2 that comes off the reaction, just remember to put in a suck back trap and use heaps of ice to keep it cool or it will over heat and waste all that valuable no2.. peroxide helps and so does having a bubbling container with a big enough mouth to drop ice directly in the weak nitric because it will get hot fast and it's hard to keep it cool.. from there it's easy to distill to make 68 percent out of the no2 coming off the reaction.. i forget the yield off hand but it is well worth the extra trouble, once processed it's well over 250ml of 68percent just from catching no2
When using the dry method, how long of a time-line does it take to produce the nitric?
solder had also not helped with the temperature sensors, the connection wires of such sensors are made of platinum or platinum/nickel so that the set resistance of 100, 500 or 1000 ohms is not affected, such connections are either spot welded or crimped, Actually, the entire connection up to the PCB should be made of platinum wire, which is also the reason why high-quality RTD sensors with only two very long connections are very expensive
Drywall screws in osb. Monster detected.
❤❤❤❤
Oleum to sulphuric acid next?
you could just use the working sensor and hotwire/jump the other.
You said that sulfuric acid is hard to get but is there a problem with simply distilling drain cleaner? Assuming you get a good source.
Not every country sells drain cleaner sulfuric acid and not every country can sell sulfuric cheap or even at a higher concentration than 15%. Its also stupidly dangerous to distill sulfuric acid
also it is expensive to take a gallon of drain cleaner and purify it down to anhydrous concentrations and still have to deal with contamination. The difference between lab grade and toilet grade can mean the difference between failure and success or full yield and a random yield. Considering the end product of this was nitric acid there are easier methods to make nitric acid but easy is not the point of this the science is. For that matter easier ways to make sulfuric auto parts stores could carry it to refill car batteries.
Any tip on dealing with HCLO4
The hotplate is gradually transforming into a Ship of Theseus, or Trigger's Broom, whichever side of the education spectrum you reside upon... :P
I got an Agilent Technologies ad on this video. I find that amusing because my dad works at Agilent as a contractor who programs for one of their logistics centers.
Awesome work. I have two questions if you have time.
1. Could heating the 5(Ca(NO3)2)*NH4NO3*10H20 at ~150C prior to adding the NaHSO4 drive off the water, leading to a higher % HNO3?
2. The pool pH lowering chems I find locally are labeled as 93% NaHSO4. Do you have any idea what the inerts are, and if they would interfere with the reaction?
1. it probably would, but at the cost of lower yield, the water helps to solubilize the reactants so the reaction goes to completion.
2. likely Na2SO4, and that would not interfere, just use an excess
@@NurdRage Awesome thanks, I'll join your patreon. Also would love so see the updated nitric acid guide at some point.
@@NurdRage What was the approximate concentration of the acid produced from the dry method?
I can hope that your crappy repair job doesn't fail after more than just a few uses of the hot plate
Concentrated Hydrochloric acid should dissolve all the calcium deposits in the flask so that should not be a problem.
Can sodium sulfate be used instead of bisulfate,, or can smb be used too.. which is best or most effective to make nitric acid
no
Is it possible to start with more complex chemicals and decomposing them instead of starting with less complex chemicals and constructing them?
no easier methods starting with more complex chemicals
what, you don't have some chonky 2500uF capacitor flying around? Those things can make microwelds like champs.
For some reason I never get you notifications despite clicking the bell and selecting all.
I honestly feel the best choice when using calcium (ammonium) nitrate is to mix a solution of it with ammonium solution. it will form insoluble calcium hydroxide and ammonium nitrate. You can even use excess ammonium solution to ensure full conversion of the calcium salt then recapture the excess ammonia. it is a little extra work but it is much easier to make nitric acid with pure ammonium nitrate than calcium nitrate or the mixed salt.
You can than easily form sodium/potassium nitrate with the appropriate alkali hydroxide. This can be done from the mixed salt too but you will always have either a calcium nitrate or alkali hydroxide impurity which could hinder some reactions. Yes you will have the same issue with pure ammonium nitrate but just use and excess of ammonium salt and the impurity will be guaranteed to be ammonium nitrate and not the alkali hydroxide. For most reactions a small ammonium nitrate impurity will not affect the reaction in the same way calcium nitrate or alkali hydroxides will. Also when drying the alkali nitrate a byproduct will be ammonia gas which can be recaptured helping replenish the supply you used in the initial reaction.
Yes it is more work but you have a higher rate of success in your reactions, and you will not end up with nasty gypsum in your flask.
calcium hydroxide is soluable in water
@@EdwardTriesToScience it is very slightly soluble, and the solubility decreases with an increase in which is opposite the normal solubility rules. As soon as the temperature starts to rise CA(OH)2 starts dropping out.
If you don't remove it, it will contaminate your product.
you can use NaCl to destroy the calcium sulfate
Is ti possible to use acetic acid? Calcium acetate is pretty soluble.
no
I live in Algeria where I cant find any trace of nitrates or nitric acid otc
Is there anyway that you can make nitrates with urea or ammonia or something that would super awsome
أه كاينا طرق باش تصاوب حمض النتريك
ua-cam.com/video/ep23ds4cZs4/v-deo.html
@@shadowshadow2724 how?
@@KainYusanagi check out codys lab he makes it with a pickle jar and high voltage electric arc and seemed possible to do at home. The link above is the video I'm referring to.
@@Rich_ard ...Dude. That's literally the Cody's Lab video I linked because of his question. I obviously do watch Cody.
I'm wondering if this process works equally well with CaNO3 instead of CAN or if it even matters. I can get as much CaNO3 as I want dirt cheap but CAN is a different animal.
can works
@@user-ir2tm6vg3c "can works"
Bro you confused me with that Message.
Does IT Work??😂😂😂❤
@@prolethazine6293 CAN is short for calcium ammonium nitrate the latter is calcium nitrate -- they both work.
May I ask someone if I can make silver nitrate from electrolysis of a sodium nitrate solution with silver and graphite electrodes ?
I don't have any nitric acid or sulfuric acid, so I thought this method would work. I'm thinking of building a separate cell for each electrode, so that the sodium hydroxide formed on the cathode doesn't react with the silver nitrate (something like a simple membrane cell).
Can someone help me with this project ?
I think that could work if you used a membrane cell. I dont have enough experience or knowledge to tell you for sure, but as long as you can do it in a safe spot (Hydrogen gas, and potential Oxygen gas) outside it's worth a try.
@@theprogrammer32 Thanks !
If your copper leads stop working try some silver solder with a high enough melt temp. And, I have a bag of calcium nitrate and some sodium bisulfate and will give it a burl.
Cheers, Mark
**************************
Please make a video on all the options for making Nitric Acid for those of us unable to buy most of the ingredients you mention. Anything remotely fun is banned.
To buy Nitric Acid here we need to apply to a licence from the Government at extortionate costs. I only want a bit to copy some experiments with copper and gold.
Thanks for the videos though.
bruh CAN is available even in strict places just look around more. If worse comes to worst electrolyze air: ua-cam.com/video/ep23ds4cZs4/v-deo.html
too bad it was not the heating element that broke, you have like 27 of them left.
(Just en fyi you have this high temperature heat shrink you can add to the joints, just to make sure nothing gets shorted.)
or do it the classic old school way and just spiral the wires together. Good enough for high power transmission lines and reliable communication lines! Lineman's Splice
I bet Big Clive could fix it. Not only fix it, but power it up to have ludicrous abilities.
Isn't it Sodium Nitrate rather than Sodium Sulfate which is remaining with the Calcium Sulfate?
cano3 + nahso4 ---> hno3 + na2so4 + caso4
Buy terminated sensors with incorporated wires. If you need the special terminal, just cut them off and solder them back on far from the heat source. You can use a high temperature solder for a higher safety margin.
Also, I thought there'd be some kind of high-temperature solder that'd survive 400C. Then again, how the hell does a chemist solder something at that temperature?
There is solder for that temp range but the part won't survive the soldering. Spot welding works because it's so very fast.
Hey 👍 Can you tell me how can I make Kclo³?
boil down bleach and add kcl or electrolyse kcl
where did you get that hot plate it seems robust as hack! after what? ... only 5 years you fixed it twice? considering of how you abuse that plate its remarkable! i want one. that would be a good product review with a serious testing of the product 😏
Are you sure you don't just have asbestos fingers?
Good call on the foil. My dumbass would have tried to solder it.
you can use microwave , get 3 glass were the fits inside each then add aluminum (lead is better but it's toxic) in the smallest one and water in the next or (NaOH solution to get NaNO3) and turn the microwave on the plasma will do it for you , i use solar panel so it's kind free for me to make , i use it to fireworks aluminum is explosive so it help the reaction ...
how long do you run it for what yield?
Can you uncover Mark Rober’s secret “Devil’s Toothpaste” formula??
From how the chemicals looked im guessing it the normal elephants toothpaste stuff (KI & H2O2) but heated up since i saw that liquids were steaming when they poured it.
bruh it's just 30% h2o2 instead of 3% how is this not obvious?
I just discovered that I had been unsubscribed from you, what's up with that youtube!?
Which chemical does not seen in mirror
????????????????????????????????????????????????????grammer
Are you NileRed's pep-pep?
I know you will ignore this comment. (._.) But pls. Read and reply
Hey , nurdrage I am a fan of yours and follow cool stuff of yours and some other cool channels like nile red. I also do many complex reactions but there is a strict oppose for chemistry at my damn home in India. By the way, you are just GREAT. Bye. Waiting for YOU to reply
You can get small wire crimp connectors designed for exactly this. Here's a digikey link for one for 15-22 AWG wire that looks like about the size you have there. www.digikey.com/product-detail/en/te-connectivity-amp-connectors/170152-3/A117873CT-ND/4729981
Hi
4:01 That's why I always recommend to buy MADE IN INDIA😊😊✊🏻✊🏻🇮🇳🇮🇳
Create a video Composition of crystal meth and its ingredients?????
lol
Just use a bootlace ferrule and crimp it with a pair of pliers. See e.g. i.ebayimg.com/images/i/321293964198-0-1/s-l1000.jpg