| Pages:
1
..
18
19
20
21
22 |
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
Quote: Originally posted by Hawkguy  | | Dude it'll be easier to go all out with fermenting grass right away on a large scale, instead of wasting time on small trial runs. I'm finding out now
that it looks like about 1 to 2 years before much can be produced by this method on a reasonable scale. |
I am surrounded by farms! Plenty of silage pits around here, so the plan is too go get some silage from deep in a pile and mix with some maggot juice
(as a trial) and see what I can do. I have something in mind................
The main problem is I have always lived around farms and never seen that before, so I asked my dad about it. Apparently many places like where we
lived and where we now live are nitrogen sensitive areas. So there are strict limits on how much nitrogen you can put on a field, I suspect that this
keeps the nitrogen levels in grass pretty low around here.
But if its starting to ferment then maybe adding in nitrates or ammonia will help kick it off, I have access to small bioreactors (1 ltr) so it might
be worth seeing what happens if I help it with some heat in the jacket.
Maybe grass is the wrong material, there are alot of plants much higher in nitrogen (comfrey), I know in bio gas plants you can get hydrogen sulphide
if it goes wrong. Maybe cow poo in a reactor under the right conditions would push things over to NOx gases?
Obviously I am wildly guessing so please jump in with sugestions
Dont ask me, I only know enough to be dangerous
|
|
|
WGTR
National Hazard
Posts: 971
Registered: 29-9-2013
Location: Online
Member Is Offline
Mood: Outline
|
|
Typically the idea is to avoid producing these gasses, so most of what I've read so far is geared towards that. This is
something that I've never tried myself, so I have little idea as to what the yield would be, or what the optimal conditions are.
Just on a whim, I added 0.9g of pulverized grass and root bits to a 3mL syringe; added 0.1g Mg(NO3)2 to 0.56g of DI
H2O,
and suctioned it into the syringe; and then carefully removed as much air from the syringe as possible and capped it.
I got quite busy this morning and forgot the syringe at home. When things slow down today I'll bring it into work and incubate
it over the weekend. In years past when I put green grass clippings into a sealed syringe (without added water), within
several hours I start seeing gas fill up the syringe. I think this was mostly CO2, and it was produced mostly in the
beginning when there was still some oxygen left in the syringe.
When I'd add water to the grass, over the next several days the pH would drop. Adding Mg(OH)2 in small amounts
after a week or so would help raise the pH, since I was trying to make methane (I succeeded at the time).
After sitting overnight at room temperature, my syringe is still sitting there quietly, without producing any obvious amount of
gas. I probably shouldn't have added water to it.
My understanding is that nitrates eventually get reduced to nitrogen, with nitrite as an intermediate step. If the nitrite
levels are high enough, and other volatile fatty acids are being produced, some of the resulting nitrous acid decomposes, with
some NO escaping from the fermentation. If the environment remains sealed, then eventually nitrogen is the end product.
Buffering the pH lengthens the time that the fermentation continues, and produces more VFAs.
I think the problem with silo gas is more likely to happen naturally in drought-prone areas. Here in Texas it's a bigger problem, I
think. It sounds like you're used to being on and around farm operations, but I'll mention it for other's benefit, that
fermentations can produce some interesting and sometimes unexpected gasses. Methane, carbon dioxide, sulfides, nitrogen oxides,
and possibly even cyanides. So, be careful. Some cattle down here got turned loose in a field that had just recovered from a
drought, and most of them died from cyanide poisoning. It turns out the grass had developed high cyanide levels.
http://www.wired.com/2012/06/cyanide-and-poisoned-cows/
I don't claim to know much about the grass fermentation process, I just play around in the lab from time to time.
|
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
| Quote: Originally posted by WGTR | Typically the idea is to avoid producing these gasses, so most of what I've read so far is geared towards that. This is
something that I've never tried myself, so I have little idea as to what the yield would be, or what the optimal conditions are.
Just on a whim, I added 0.9g of pulverized grass and root bits to a 3mL syringe; added 0.1g Mg(NO3)2 to 0.56g of DI
H2O,
and suctioned it into the syringe; and then carefully removed as much air from the syringe as possible and capped it.
I got quite busy this morning and forgot the syringe at home. When things slow down today I'll bring it into work and incubate
it over the weekend. In years past when I put green grass clippings into a sealed syringe (without added water), within
several hours I start seeing gas fill up the syringe. I think this was mostly CO2, and it was produced mostly in the
beginning when there was still some oxygen left in the syringe.
When I'd add water to the grass, over the next several days the pH would drop. Adding Mg(OH)2 in small amounts
after a week or so would help raise the pH, since I was trying to make methane (I succeeded at the time).
After sitting overnight at room temperature, my syringe is still sitting there quietly, without producing any obvious amount of
gas. I probably shouldn't have added water to it.
My understanding is that nitrates eventually get reduced to nitrogen, with nitrite as an intermediate step. If the nitrite
levels are high enough, and other volatile fatty acids are being produced, some of the resulting nitrous acid decomposes, with
some NO escaping from the fermentation. If the environment remains sealed, then eventually nitrogen is the end product.
Buffering the pH lengthens the time that the fermentation continues, and produces more VFAs.
I think the problem with silo gas is more likely to happen naturally in drought-prone areas. Here in Texas it's a bigger problem, I
think. It sounds like you're used to being on and around farm operations, but I'll mention it for other's benefit, that
fermentations can produce some interesting and sometimes unexpected gasses. Methane, carbon dioxide, sulfides, nitrogen oxides,
and possibly even cyanides. So, be careful. Some cattle down here got turned loose in a field that had just recovered from a
drought, and most of them died from cyanide poisoning. It turns out the grass had developed high cyanide levels.
http://www.wired.com/2012/06/cyanide-and-poisoned-cows/
I don't claim to know much about the grass fermentation process, I just play around in the lab from time to time. |
Really really interesting thanks for the information.
I might just be able to add a couple of things, grass and silage here spoils because it gets too wet, so when cut they dry to leave around 30%
moisture (thats practice and not science test) what the farmers do is cut and turn but pick up a day or so before they would for hay.
This gives you enough moisture to ferment without spoiling and producing hydrogen sulphide. No one has ever mentioned the nitrogen gases to me and dad
who has lived on and around farms all his life hasnt heard or seen it. He is also a Biologist, he thinks that because in the uk they are very strict
on the amount of nitrates you can spread on grass in many areas this would account for the lower nitrate in the grass here.
We have the rules for the nitrates levels because of the damage they can do to the river systems etc with algae blooms (uk is very wet and it washes
into water courses).
I am also trying the grass fermentation, but first I am giving it two days of free air but a little heat (26c), i chose this because I figured the
stage would need air like a silage pit does, then its closed up to exclude most the air, in practice the farmers I know wait for the pile to drop a
couple of feet then they seal the pit off (this is called a clamp in the uk), its different from the wrapped bales but gives much better feed. So I
figured I would compact the grass a bit and wait till the level drops a little then seal up.
I might also add cow shit (tiny amount) as going the methane route as a start point is a good idea.
I am going to use one of these
at the moment my grass is in a plain glass jar, but once it starts to do something I can transfer to the fer mentor. it should give me good control
over the fermentation and i can add buffers ect via the septum or one the tubes. It also has a stir thing and any gas evolved could be piped into this
I might add some form of wet sugar like honey or malases (again tiny amount). i will let you know if anything happens. If it start to ferment I will
up the temperature to around 30C, I found out methane ect should stop at 40c, this was from a bio gas page about a car in the uk running from the gas
made from chicken shit back in the 70's, I will try and find the page again
Dont ask me, I only know enough to be dangerous
|
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
I will see what I can find on methane production, I know the nitrate cycle very well because I have kept fish from a very early age  . I have seen aquariums go really bad (not mine) and produce hydrogen sulphide and
the water goes a funny red black colour, this normally happens when a fish keeper goes away for two weeks and a friend feeds the aquarium with way too
much food.
So I might add a little more maggot juice to the jar, i am thinking that in a dryer environment than an aquarium the sweet spot would be just before
the hydrogen sulphide stage. Soooo this means fermentation and bacteria converting Ammonia - nitrite-nitrate then suddenly large increase in ammonia
so the bacteria are overwhelmed a fair bit.
I honestly dont know what to expect as i have always tried to keep the cycle going right, I know if you close off early and dont have fermentation
started you get methane, so somewhere between the two should make nitrogen gases, also in older aquarium systems they used a column that was dripped
fed alcohol at a tiny rate and this converted the nitrate to nitrogen, it was the in thing ages ago until people got more into CO2 injection and
nitrate stripping via plants (they do it really really fast under the right conditions).
Anyway time to stop waffling and see if I can track down some leads.
I might start at bio gas production and this could possibly go wrong and produce nitrous gases if the conditions are wrong?
Dont ask me, I only know enough to be dangerous
|
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
found this.... http://www.nature.com/news/2010/100324/full/news.2010.146.ht...
Probably no use what soever but interesting considering the topic.
having read the original link again and going to the site about silage I can see some big difference between what they do and what I have seen done in
both England and Scotland. I have no idea how helpful this is going to be though. The Uk has mainly two different ways of making silage, what is shown
in the link with the brown gas is crosser to what we would call a silage clamp, these are pretty much like compost heaps that are allowed to heat up
for a couple of days then sealed off with a covering.
The product from this is rich smelling and slightly damp, I cant describe the smell but it isnt unpleasant. I know its pretty high in sugars as it is
normally used to supplement feed and just before calving time ect.
The other and probaly now the more common way is just like making hay except you harvest it very slightly moist and its wrapped air tight by the
machine that bales it. These large bales are very common here and seen as black plastic large round objects all over fields in the uk (its being cut
and done right now actually), this type of silage is much more dry and is used more as a general feed through out the year.
It also seems fields here are nitrated at different times to over there, in the uk ferts are spread just after the last cut of the year, then just
before new spring growth then on occasion after the first cut.
I cant think of nor have I seen any situation where in the uk they would spray or use nitrates near a cut period, mainly I think because its cut
during dry spells and it wouldnt make much sense to spread it then, plus also nitrate run off is highly controlled in both areas I have lived in.
But its really interesting to read the silage site and see the difference in the feedstock. I wonder if cattle breeds play a part? i think that amount
of sugar and nitrate would bloat most breeds of british cattle, I know we cant have the ponies out on the spring or early grass because of the sugar
content.
Funny I have grown up around farming but grass has always just been green stuff to me lol.
[Edited on 4-9-2015 by Little_Ghost_again]
Dont ask me, I only know enough to be dangerous
|
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
Ok out of desperation mainly I came upon this but I am not sure its plausible, maybe I am just tired! Anyone want to comment on this?
https://www.google.co.uk/patents/US8327581?dq=making+nitric+...
The one thing i have totally overlooked is the reaction vessel, as you can see its mainly stainless steel! I have a busted glass version that I might
be able to fix enough to use, the down side being it dosnt have a stiring mechanism so I would have to use normal stir plate and bar, I dont think
that will work though.
I am not so much after the prize (although that would be great) But this has really caught my imagination once I got over the thinking of normal
routes.
I now kind of see the point of this challenge
[Edited on 5-9-2015 by Little_Ghost_again]
Dont ask me, I only know enough to be dangerous
|
|
|
WGTR
National Hazard
Posts: 971
Registered: 29-9-2013
Location: Online
Member Is Offline
Mood: Outline
|
|
It's an interesting document, but I think it's referring to nitrates rather than nitric acid per se.
I hope it's possible to get good yields of NO from fermentations, but the approach might turn out to be a dead end, or not particularly high-yielding.
That's an unfortunate possibility in research.
I'm still working on Dead Woodchuck. It's become much more refined, characterized, and...well...interesting than before. I spent the whole weekend 3D modelling
different parts of it. It took so long, not because of the sheer volumes of work that I did on it, but because I'm a Solidworks beginner. I think
that a beginner can do almost anything with Solidworks that a professional can do, due to the helpfulness of Youtube tutorials. A beginner, though
(me), will probably take 10 times longer at the job than someone who knows what they're doing (not me).
I'm modelling everything before I build the final revision, but the latest prototype tests went well. The design still uses a high voltage pulse to
trigger the main discharge. The amount of energy supplied by the high voltage is a small amount of the overall discharge, and is calculated to be
within safe limits. The main arc current is supplied from a 65V power supply. Peak power is about 500W at 10A, but due to low duty cycle the average
power is about 6W. This high peak power made it a challenge to design the filter network. All of the parts run cool to the touch, including the
copper reactor tube and the electrodes, which are cooled with a small fan.
It's not really a contender for the competition since it uses a high voltage trigger, but it's a fun project nonetheless.
|
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
I think thats pretty neat! I can get to hydrogen sulphide really easy. That paper was a bit misleading but I have others that say something similar, I
cant see it though. The only thing that makes me wonder its possible by fermentation is the fact methane reactors can suffer from NOx gases, I have to
spend the next two days catching up on school work Grrrrr
Dont ask me, I only know enough to be dangerous
|
|
|
no0ne98
Harmless
Posts: 1
Registered: 10-10-2015
Member Is Offline
Mood: No Mood
|
|
I don't know that this will fall under the challenge rules. However it's a good read that even covers nitric http://www.pyrobin.com/files/the_manufacture_of_chemicals_by...
|
|
|
j_sum1
Administrator
Posts: 6334
Registered: 4-10-2014
Location: At home
Member Is Offline
Mood: Most of the ducks are in a row
|
|
It's a nice reference.
|
|
|
aga
Forum Drunkard
Posts: 7030
Registered: 25-3-2014
Member Is Offline
|
|
Which part of the Voltage Rule, or the workings of the Birkland-Eyde Process did you not read, look up or understand ?
Can somebody please complete this challenge soon, so we can get on with the AntiGravity Challenge ?
|
|
|
j_sum1
Administrator
Posts: 6334
Registered: 4-10-2014
Location: At home
Member Is Offline
Mood: Most of the ducks are in a row
|
|
Hey. I was just looking at my manganese-coated peanuts the other day.
I have everything I need and I need the bench space back so it will happen.
However, weekends are booked out for the next month and after that is crazy time at work. Then holidays. I might have a result by Christmas.
|
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
need to scale up and do pics so it can be verified. Turned out I was over thinking it
HOLD ON
I think its nitrous acid 
[Edited on 12-10-2015 by Little_Ghost_again]
Dont ask me, I only know enough to be dangerous
|
|
|
j_sum1
Administrator
Posts: 6334
Registered: 4-10-2014
Location: At home
Member Is Offline
Mood: Most of the ducks are in a row
|
|
Wohoohoo LGA. Looking forward to seeing it.
|
|
|
Little_Ghost_again
National Hazard
Posts: 985
Registered: 16-9-2014
Member Is Offline
Mood: Baffled
|
|
How do I check between nitrous acid and nitric?
Foof it I will take some and distill and see if it fumes red, man I wished I had my old fume hood working lol
[Edited on 12-10-2015 by Little_Ghost_again]
Dont ask me, I only know enough to be dangerous
|
|
|
hamdusf
Harmless
Posts: 2
Registered: 26-10-2015
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by j_sum1 | Hey. I was just looking at my manganese-coated peanuts the other day.
I have everything I need and I need the bench space back so it will happen.
However, weekends are booked out for the next month and after that is crazy time at work. Then holidays. I might have a result by Christmas.
|
there is new way of make nitric acid
[Edited on 27-10-2015 by hamdusf]
|
|
|
aga
Forum Drunkard
Posts: 7030
Registered: 25-3-2014
Member Is Offline
|
|
Let me Guess !
#1 zap the air wth a high voltage arc
#2 distill a nitrate with concentrated sulphuric acid.
Oh the excitement.
|
|
|
Grantr
Hazard to Self
Posts: 57
Registered: 19-9-2015
Member Is Offline
Mood: No Mood
|
|
I know scrubbing exhaust was mentioned however I did not see reference to diesel.
Diesel exhaust has a high level of NOX due to lean hot combustion.
In the article below, The 2000 Volvo produced 112.5 grams of Nox in an hour idling at 1000 rpms and consumed .8 gallons of fuel. That seems like a
good bit of nox.
http://nepis.epa.gov/Adobe/PDF/P10033E3.PDF
|
|
|
deltaH
Dangerous source of unreferenced speculation
Posts: 1663
Registered: 30-9-2013
Location: South Africa
Member Is Offline
Mood: Heavily protonated
|
|
| Quote: Originally posted by Grantr | I know scrubbing exhaust was mentioned however I did not see reference to diesel.
Diesel exhaust has a high level of NOX due to lean hot combustion.
In the article below, The 2000 Volvo produced 112.5 grams of Nox in an hour idling at 1000 rpms and consumed .8 gallons of fuel. That seems like a
good bit of nox.
http://nepis.epa.gov/Adobe/PDF/P10033E3.PDF |
Yes, though the concentration would be much lower than burning fuels that also contain nitrogen in their structure and at such low concentration, it
might be hard to capture/concentrate it out of the total exhaust volume.
What would the exhaust volume be for a 1h idle? It's easy to calculate and then back calculate the ppm NOx given your figures.
|
|
|
Agari
Banned
Posts: 160
Registered: 8-10-2015
Location: The Amine Group
Member Is Offline
Mood: Lowest Oxidation State
|
|
Materials:
1 Instand cold pack (Either 86g of calcium ammonium nitrate or just 70g of ammonium nitrate), but not urea.
75g of potassium chloride bought at a grocery store.
Procedure:
Cut open the cold pack and isolate the nitrate contained.
Add the nitrate salt to a beaker.
Add 200 milliliters of water.
Stir the mixture until it has fully dissolved.
Gravity-filter the mixture into a beaker.
Heat the solution in the beaker to near-boiling (I did not record temperature) and add the potassium chloride.
Bring the solution to a boil(with stirring!) and gravity-filter it into a beaker.
Place the solution in a home freezer to precipitate as many Potassium Nitrate crystals as possible.
Carefully remove the upper water layer from the beaker,then recrystalize the remaining KNO3 crystals from water.
Freeze the solution again.
If done right,the result should be white potassium nitrate crystals and yellow-ish water on top,remove the water and wash the crystals with ice-cold
distilled water (Available at Walmart).
Dry out the crystals on a watch glass.
Nitric Acid Preparation:
Materials:
110 grams of Potassium Nitrate obtained previously.
Copper Sulfate.
Dissolve the copper sulfate in water.
Next,extract the carbon core from a single battery and attach a copper wire to it,connect our home-made electrode to the positive terminal of a power
supply such as a battery.
Next,place a copper electrode at the bottom of the copper sulfate solution and connect it to the positive terminal of the battery. Suspend the carbon
electrode above the copper electrode,make sure they do not touch!
If the carbon electrode erodes to the point of the solution becoming almost black,filter it out and subject the remaining solution to the same cycle
using a different carbon electrode until it is clear. Once the solution IS clear,remove both electrodes,the liquid should be sulfuric acid.
Alternatively,battery acid can be purchased at an auto-shop and distilled to maximum possible concentration, just writing
that in case copper sulfate is prohibited.
I only used 60 milliliters of acid for my batch.
Now that we got sulfuric acid and potassium nitrate,it is time to prepare nitric acid.
Mix the potassium nitrate and sulfuric acid in a round-bottom flask in that order and (maybe?) add boiling stones.
Set up a simple distillation with the receiving flask placed in an ice bath and cover the entire apparatus with aluminum foil.Now bring the mixture to
a boil at 83 degrees Celsius,continue the distillation until no liquid remains in the flask that used to contain potassium nitrate and sulfuric acid.
Repeat the entire above process until 100 milliliters of nitric acid is obtained. I did not wear gloves during the experiment as the acid is likely
concentrated to fuming(and likely to ignite the gloves), but rather has a solution of sodium bicarbonate and water nearby in case of contact with the
acid.
Edit 1:I got around 25ml of nitric acid per run.
[Edited on 30-10-2015 by Agari]
[Edited on 30-10-2015 by Agari]
[Edited on 30-10-2015 by Agari]
Edit:
Alternative method for making nitrates:
Obtain a tub of composted turkey manure (highly composted mixture of woodchips and turkey feces),6 kilograms is what I plan to use. Then add 4 liters
of water,stir it with either a rod or manually. Then,gravity or vacuum filter the resulting mixture into a tub,discard to left-over insoluble material
in the filter.Add a quart of a water and sodium carbonate solution at maximum concentration at room temperature. Boil off the resulting fluid ,do not
include the precipitated calcium waste at the bottom of the tub in the boiling process. Next,reddisolve the left-over nitrate crystals in water.
Gently boil the solution until the organic material precipitates at the sides of the container used to boil the solution,leaving a layer of nitrate at
the bottom. Redissolve everything in water again,then use a separatory funnel to separate the darker nitrate layer from the lighter nitrate layer.
Boil off the lighter layer. The resulting salt is now mostly nitrate,yet heavily contaminated.Do the same for the darker layer. Add just enough water
to completely dissolve the salts.Mix the two solutions.
Boil off the nitrate extract,the potassium nitrate within should crystalize while other contaminants are largely in solution. After the boiling,place
the resulting fluid in a freezer to further preipitate the nitrate,but not to freezing point. After 2 hours,remove the container with the fluid,there
should be a layer of liquid above the nitrate crystals,decant and discard that liquid. Dry the crystals in the container on a watch glass with a paper
towel to soak up the water. Do not hesitate to use water to remove the crystals,they will be dried anyways.
Alternative to Sulfuric Acid(This method must be performed with gloves,a respirator,and under a fume hood or outside):
Firstly,pplace 16 grams of dried sulfur powder in a beaker, then add a raft electrode consisting of 5 carbon battery cores, suspend the electrode
above the sulfur,make sur ethey do not touch. This will be our anode. For the cathode,use a copper wire suspended below the top of the beaker.
Now,use alligator clips to connect the electrodes to a car battery or other power supply,positive terminal for the anode,negative for the cathode.
Next,add 200 ml of a 5 molar solution of hydrobromic acid to the beaker. Make sure that the carbon electrodes are sumbmerged at least 5 CM below the
surface of the electrolyte(HBr) and that the cathode is under the surface of the electrolyte but at least 2 centimeters above the sulfur powder. Turn
on your power supply and set the current to 2 amps. Should some sulfur start floating during the electrolysis process,stir the liquid until it is
submerged. Water additions may be required should one electrolode end up too close to the surface. Run the electrolysis for 2-3 hours. After removing
the electrodes,stir the mixture to dissolve all substances within and transfer it to an Erlenmeyer flask. Next, set up a reflux apparatus above the
mixture and boil(With a hot plate)and reflux the liquid for half an hour. Then,stop heating and cooling and use a coffee filter to gravity filter the
resulting fluid into an Erlenmeyer flask. Set up a simple distillation apparatus with stirring and heat the Erlenmeyer to 154 degrees Celsius until
misting in the flask occurs and no more distillant comes over to the collecting beaker/flask.
Now,we must purify the sulfuric acid for it to be usable. Since most ehating mantles don't reach temperatures high enough to boil H2SO4,we must
build one. For the mantle,we must unfortunately firstly buy special heating tape,I bought mine from Omega Engineering,model number STH051-040.
Roll up the tape and mold it into a cup shape to be able to accomadate a 100 ml round-bottom flask,you can use larger sizes to suit your needs. Once
you have a satisfactory shape,use iron wire to hold the tape in place and maintain shape. Now,place the home-made mantle in a steel thermos to prevent
heat loss during heating,then bend the iron wires to support the heating tape. Unfortunately,when the power cord is plugged in,there will be no way to
regulate the current and the mantle will heat up at full power. To correct this issue, use either a light dimmer switch or a PID controller,but I had
to buy a Variac auto-transformer for power control.
Now that our heating mantle is all set up,we can distill the sulfuric acid, a simple distillation apparatus with cooling(I actually used dry ice to
keep the water cool) will do. The flask with the dark solution obtained from the simple distillation during our sulfuric acid synthesis must be
connected to the condenser using high-temperature grease,normal grease will not work,it is also best to use high-temperature grease for the receiving
flask for safety reasons. Next,turn on the heating mantle at low power and gradually increase voltage until condensate begins to come over into the
collector. An important fact worth noting is that the flask wit the unclean acid must be filled only halfway,as thermal expansion will occur at such
high temperatures. Due to water contaminating our distillant,we must collect when the concentration of H2SO4 is highest. To test the concentration,use
a pippete to sample the distillant in the receiving flask and apply it to a paper towel. If nothing happens,the sulfuric acid concentration is still
low and the contaminated distillant should be discarded. Keep performing this test until your paper towel begins to burn. Change the receiving flask
to start collecting nearly pure sulfuric acid. Though our acid is highly concentrated,it is still not 98%. To determine when the acid concentration is
at 98%,watch the receiving flask/beaker carefully. If the acid concentration is increasing,there would be oil-like patterns in the solution. Once this
occurs,change out the receiver so that only the most highly concentrated sulfuric acid will be collected. Run the distillation until only 20% of the
crude product remains in the heated flask,continuing the distillation after this point is likely to contaminate our concentrated acid. To create
nitric acid,simply follow the original procedure once enough nitrate salt and sulfuric acid is obtained.
Before Aga calls me out on hydrobromic acid not being a common chemical, I am going to write a synthesis procedure for it as well.
Note:Use a conventional hot plate for this process,not the cutsom heating mantle built previously.
First,add 300ml of a 35% solution of sodium bromide(Available in pool stores) to an appropriate beaker,next add a stir bar and begin stirring rapidly,
then add 200 grams of sodium bisulfate(Also available at pool stores),stir and heat until the sodium bisulfate dissolves. Once everything is
dissolved,turn off heating and let the mixture cool to room temperature,then place the beaker in an ice bath. The products produced by the above
reaction are sodium sulfate and hydrobromic acid. The ice cooling will precipitate the sodium sulfate out of solution. After an hour,remove the beaker
from the ice bath and use a coffee filter to gravity filter the liquid into an Erlenmeyer flask,discard the remaining sodium sulfate crystals. To
further purify the HBr,set up a simple distillation apparatus and distill off the hydrobromic acid.
Preparation of Nitric Acid.
Mix the nitrate salt and sulfuric acid in a round-bottom flask in that order and (not neccessarily) add boiling stones.
Set up a simple distillation with the receiving flask placed in an ice bath and cover the entire apparatus with aluminum foil.Now bring the mixture to
a boil at 83 degrees Celsius,continue the distillation until no liquid remains in the flask that used to contain potassium nitrate and sulfuric acid.
Repeat the entire above process until 100 milliliters of nitric acid is obtained. I did not wear gloves during the experiment as the acid is likely
concentrated to fuming(and likely to ignite the gloves), but rather has a solution of sodium bicarbonate and water nearby in case of contact with the
acid.
Pics soon to follow.
[Edited on 31-10-2015 by Agari]
|
|
|
Agari
Banned
Posts: 160
Registered: 8-10-2015
Location: The Amine Group
Member Is Offline
Mood: Lowest Oxidation State
|
|
I did not specify quantities because I did not record them during the production of sulfuric acid.
|
|
|
aga
Forum Drunkard
Posts: 7030
Registered: 25-3-2014
Member Is Offline
|
|
Ooooh !
Sulphuric acid and a Nitrate Salt !
I fart in your general direction.
|
|
|
j_sum1
Administrator
Posts: 6334
Registered: 4-10-2014
Location: At home
Member Is Offline
Mood: Most of the ducks are in a row
|
|
To clarify, Agari...
Aga has specifically excluded readily available nitrated from this competition. The H2SO4/nitrate route is well known. The comp is for a novel route
that is accessible to a wide range of people. Although long, the whole thread is worth a read. There have been a number of novel routes proposed.
The execution of them remains a challenge. This comp is not as easy as it first appears -- if only because fo the investment of time to make
progress. That said, the French Method, which was proposed early would be a viable method for nitrate production. It takes a long time and to my
knowledge, noi one has actually attempted it. If they had, they would be well ahead of the pack by this stage.
|
|
|
Agari
Banned
Posts: 160
Registered: 8-10-2015
Location: The Amine Group
Member Is Offline
Mood: Lowest Oxidation State
|
|
| Quote: Originally posted by j_sum1 | To clarify, Agari...
Aga has specifically excluded readily available nitrated from this competition. The H2SO4/nitrate route is well known. The comp is for a novel route
that is accessible to a wide range of people. Although long, the whole thread is worth a read. There have been a number of novel routes proposed.
The execution of them remains a challenge. This comp is not as easy as it first appears -- if only because fo the investment of time to make
progress. That said, the French Method, which was proposed early would be a viable method for nitrate production. It takes a long time and to my
knowledge, noi one has actually attempted it. If they had, they would be well ahead of the pack by this stage. |
However,our drunkard implies that it is fine to MAKE the H2SO4 and nitrate salt:
| Quote: Originally posted by aga | You can't just Buy sulphuric acid, nor nitrate-based fertilizers to then go down the well-trodden 'distill to get conc nitric' route.
Even I could do that, so it would certainly not be challenging to you.
If you were to Make Sulphuric, concentrate it, and Make Nitrates, then distill, that'd be more like it.
The 'can't buy pure chemicals rule' does not include table salt, water, vinegar, booze, fags, hamburgers - stuff like that.
Bat guano would be fine, so long as the process includes details of where you might find bat dung.
Presumably in the Bat Cave, all over the Bat Mobile's windscreen.
|
The quote of relevance is "You can't just Buy sulphuric acid, nor nitrate-based fertilizers to then go down the well-trodden 'distill to get conc
nitric' route.
Even I could do that, so it would certainly not be challenging to you.
If you were to Make Sulphuric, concentrate it, and Make Nitrates, then distill, that'd be more like it.", he is suggesting that it is OK to make the
sulfuric acid and the nitrates,just not buy them.
Edit:the chemicals can also be bought at grocery stores,almost as easily as sodium chloride salt. Funny enough,my method seems to be a perfect fit for
his "Exception policy" yet he dismisses it. Fuming nitric acid is mostly used for explosive synthesis,but can be diluted for more practical purposes.
[Edited on 31-10-2015 by Agari]
|
|
|
j_sum1
Administrator
Posts: 6334
Registered: 4-10-2014
Location: At home
Member Is Offline
Mood: Most of the ducks are in a row
|
|
Ok. But it still does not qualify as a novel route. Convenient? yes. Novel? no.
Prohibited within the terms of the competition? you'll need to ask aga that. But I would read into his above comment that something a bit more
adventurous is required. After all, it is a hefty prize pool and I think you have to earn it.
|
|
|
| Pages:
1
..
18
19
20
21
22 |
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
