symboom
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Is the mad science report newsletter ready to be added to prepublication
Mad Science Reports
The art and science of amature experimentalism
[sciencemadness logo]
Quote by: Chemetix
Physicists take their superiority from working with first principles and mathematical logic. Chemistry gets its results from the messy chaotic world
of reality
Building a Amature Chemistry Lab
reagents
glassware
fumehood
NEW PROCEDURES
sodium
nitric acid
sulfur trioxide
sulfuric acid
hydrobromic acid
hydrochloric acid
HIGHLIGHTS FROM THREADS
Phosphourous
C2N14
Acetic Anhydride
FOURM MATTERS
REFRENCES
Building a Amature Chemistry Lab
Starting a lab
Basic requirements
First, one will need to choose a place generally away from dwelling space. A shed is a good choice, as it offers natural ventilation which prevents
the build-up of flammable vapors and toxic compounds. However, unless you live in a geographical area where winters are mild or non-existent, sheds or
other locations with natural ventilation may not be a good choice for your lab, as it will get too cold inside and this will interfere with various
reactions or other processes.
Furniture, like cabinets, chairs, closets, cupboards, shelves and tables are needed in the lab to store reagents and lab apparatus, as well as a
working bench for the reactions.
Reagents are necessary when doing any form of chemistry. Important reagents include:
Acids: acetic acid, formic acid, hydrochloric acid, nitric acid, sulfuric acid
Bases: sodium hydroxide, potassium hydroxide, calcium hydroxide, ammonia
Salts: sodium chloride, calcium chloride, copper(II) sulfate, potassium nitrate, ammonium nitrate, sodium bicarbonate, magnesium sulfate
Metals: aluminium, copper, iron, magnesium, sodium, zinc
Nonmetals: bromine, carbon, chlorine, iodine, phosphorus, sulfur
Organic solvents: acetone, chloroform, diethyl ether, ethanol, ethyl acetate, isopropanol, methanol, mineral oil, toluene, xylene
Inorganic solvents: water (tap or distilled)
pH indicators: phenolphthalein, methyl orange, litmus
Oxidizers: hydrogen peroxide, sodium hypochlorite
Miscellaneous reagents: charcoal, nitromethane, silicone grease, urea, etc.
Electricity and water are a must. While you can use generators if the location is not near the grid, they tend to be noisy and require fuel. You can
also rely on alternative power sources, like solar or wind, if possible.
If distilled water is required, you can hook up a water distiller to your tap water. If you cannot get water from tap, you can use barrels or tanks
full of water.
for a fuel source You can get it by either connecting to the gas grid or using propane tanks.
Your lab should be connected to a drain or, if that is not possible, to a waste container.
Disposal tanks
Corrosive or hazardous products that cannot be properly neutralized quickly, contain valuable or toxic metal ions or require special disposal are to
be stored in chemical resistant bottles, usually glass, generally in a ventilated area. These waste tanks must be properly labeled to prevent any
accidental mixing of incompatible chemicals.
NEW PROCEDURES
Make Sodium Metal with Menthol
It is a great project and achievement for the experienced amateur chemist A more efficient way to obtain sodium metal heat sodium hydroxide with
magnesium in mineral oil above 200 °C, in the presence of a tertiary or sterically bulk secondary alcohols, like t-butanol and menthol. The yield of
this route if done right can be as high as 90-95%, though the process takes hours to completion.
Make Nitric Acid by Thermal Decomposition of Copper Nitrate
Copper sulfate is reacted with calcium nitrate the resulting calcium sulfate is filtered from the solution as copper nitrate remains. This reaction
is a cheap source of nitrogen dioxide, which can be bubbled through water to generate nitric acid. The gas can also be bubbled into hydrogen peroxide
producing a higher yield
Technochemistry
Nitric acid from ammonia Oswalt style (without platnium)
Reactants used: Urea and Distilled water Catalysis NiO or CoO in support bed of Sand or red house brick Devices: Absorption tower (converted 2L sep.
funnel water with broken glass to increase surface area. Quartz Catalysis tube 8mm ID. A condenser. Air compressor. nichrome wire heating element with
insulation. This process uses a NO2 generator using urea as a source of ammonia and oxidising with air using nickel oxide or cobalt oxide on sand or
red house brick as a catalyst A condenser is used to dry the ammonia/air stream. The ammonia air mixture is fed into the reaction zone, the nice red
glow is transmitted up the quartz leads into a Quartz tube as reaction chamber. The reactor tube runs into the reaction chamber which admits air via
the custom condenser fitting. The condensate runs into a reservoir where excess gasses run to an absorption tower exhaust gasses pass into a vertical
anti suck back column before running along a small tube to the base of the tower.
Sulfur trioxide
The preparation of this compound is extremely dangerous and should only be attempted by chemists with experience working with hazardous volatile
reagents.
SO3 can be made in low yield through the pyrolysis of sodium persulfate, first forming ozone and then SOSO3. A catalytic amount of 100% sulfuric acid
is required.
Nearly the same reaction takes place when sodium bisulfate is very strongly heated, first evolving water, forming sodium pyrosulfate, which then
decomposes above 460 °C to sodium sulfate, releasing SO3.
There are reports that heating sodium pyrosulfate with concentrated sulfuric acid to 150°C results in SO3 and bisulfate.
Heating iron(II) sulfate at 700 °C with carbon yields iron(III) oxide, sulfur dioxide and sulfur trioxide. The same reaction also works with
iron(III) sulfate, at a much lower temperature, 480 °C, and produces mostly sulfur trioxide.
Pyrolysis of copper(II) sulfate above 560 °C yields sulfur trioxide and copper oxide. If the temperature gets lower, copper sulfate will reform.
Aluminium sulfate also works, though the decomposition temperature is slightly higher.
Roasting calcium sulfate with silicon dioxide (very fine sand can be used) at 1000 °C for 1 hour yields calcium silicate and sulfur trioxide. Adding
small amounts of chromium(III) oxide or tungsten(IV) oxide improves the process.[3]
Sulfur trioxide can also be obtained by oxidizing sulfur dioxide in the presence of several metal oxides, such as copper(II) oxide at high
temperatures[4] or chromium(III) oxide (at temperatures between 180-400 °C).
Adding phosphorus pentoxide to extremely concentrated sulfuric acid will release sulfur trioxide, which can be extracted via distillation.
Metaphosphoric acid can also be used instead of the pentoxide.
Sulfuric acid
A solution of copper (II) sulfate can be electrolyzed with a copper cathode and platinum/graphite anode to give spongy copper at cathode and evolution
of oxygen gas at anode, the solution diluted sulfuric acid that indicates completed reaction when it turns from blue to clear (production of hydrogen
at cathode is another sign):
When applying power, the current should be adjusted so that corrosion at the positive terminal and bubbling at the negative terminal are both
minimized. The bubbling at the negative terminal is hydrogen production and that's wasted energy that should have gone into reducing the copper
sulfate.
dilute sulfuric acid that can be boiled down to obtain concentrated sulfuric acid. It will have trace amounts of metals but for most purposes this is
not an issue.
Keep in mind that it will take a long time for the solution to go clear. if after filtering it's still blue, you'll need to keep electrolyzing it.
You'll need over 60 amp hours of current per mole of copper sulfate, and usually more since the process is not very efficient
_____
Make Sulfuric acid (metabisulfite/oxidizer method)
Sodium metabisulfite is placed at the bottom of a beaker, and 12.6 molar concentration hydrochloric acid is added. Sodium metabisulfite upon reaction
with acid will generate sulfur dioxide.The resulting gas is bubbled through nitric acid, which will release brown/red vapors. The completion of the
reaction is indicated by the ceasing of the fumes. The sulfur dioxide can also be dissolved in a hydrogen peroxide solution to form sulfuric acid This
method of oxidizing sulfur dioxide in solution does not produce an inseparable mist, which is quite convenient.
Make Sulfuric Acid by the Copper Chloride Process
Take a solution of copper (II) chloride and bubble sulfur dioxide into it until most of the copper (II) chloride is converted into copper (I)
chloride. This reaction also converts the sulfur dioxide into sulfuric acid and produces hydrochloric acid. Now the copper chloride can be regenerated
by bubbling air into the mixture until the copper chloride dissolves again. This cycle can be repeated. When you want to isolate the sulfuric acid you
forgo air infusion for that step and filter off the preciptated copper chloride. Then you distill off the hydrochloric acid and water from the
filtrate. The sulfuric acid left behind will precpitate out most of the remainig copper salts and when filtered will give you relatively pure sulfuric
acid with some water and minor copper contamination. The copper chloride can be recombined with all the hydrochloric acid from before and the cycle
repeated.
________
Sulfuric acid (electrobromine process)
make sulfuric acid from sulfur and water using electrolytically generated bromine as the catalyst.
The electrobromine method, which employs a mixture of sulfur, water, and hydrobromic acid as the electrolytic solution. The sulfur pushed to bottom of
container under the hydrobromic acid solution, then copper cathode and platinum/graphite anode are used with cathode near surface and anode at bottom
of electrolyte to apply the current. This may take longer and emits toxic bromine/sulfur bromide vapors, but reactant acid is recyclable, overall only
sulfur and water converted to sulfuric acid (omitting losses of acid as vapors)
We start with 16g of sulfur in a 250 ml beaker. We install 5 lantern battery carbon electrodes for the anode and a copper wire for the cathode. To
this setup we add 200mL of 5M hydrobromic acid. The copper cathode is readjusted to be as physically close to the top of the electrolyte as possible
while still being immersed in it. A current is then applied of less than 2 amps. The electrolysis is performed for 40 hours with occasional stirring
and addition of water to make up for evaporative loses.
Whats happening is the electrolysis converts hydrobromic acid to bromine and hydrogen. The hydrogen bubbles away and the bromine reacts with sulfur to
produce disulfur dibromide. This in turn reacts with more bromine and water to produce sulfuric acid and hydrobromic acid.
At the end of the run, the solution is filtered and then refluxed for 30 minutes to drive the conversion to completion. The solution is then distilled
to first recover water, then hydrobromic acid and finally sulfuric acid.
Hydrobromic acid
The main way of synthesizing hydrobromic acid is the reaction between alkali metal bromides and diluted sulfuric acid. Care must be taken not to use
concentrated sulfuric acid or another oxidizing acid, because these acids oxidize bromide to elemental bromine.
Hydrochloric acid
One way of synthesizing HCl is to react a mixture of sodium chloride and sodium bisulfate, or sulfuric acid. The mixture is heated and the resultant
hydrogen chloride gas is then bubbled through a solution of cold distilled water to produce hydrochloric acid.
purification crude hydrochloric acid by using the two-container technique.
The process takes a week or two to finish, and the resulting reagent-grade acid is about 5 molar rather than the 12 molar typical of commercial
concentrated hydrochloric acid. Still, it's extremely pure and concentrated enough for most purposes.
Small amounts of hydrogen chloride for laboratory use can be generated in an HCl generator by dehydrating hydrochloric acid with either sulfuric acid
or anhydrous calcium chloride.
HIGHLIGHTS FROM THREADS
Chemistry in general
Preparation of elemental phosphorus (The lesser known reactions)
Cleaned, boiled and dried chicken bones (bone meal can also be used with if used as organic firtalizer) are burned with a bunsen burner on a fireproof
surface and directly heated with the flame until they have turned into white ash. 2g of this bone ash are mixed with 0.5g magnesium powder or
activated carbon powder and 0.5g Diatomaceous earth. The mix is heated and vapors are lead underwater for the vapors to cool and condense to white
phosphorous. ---low-temperature production of phosphorus, the most interesting candidates appear to be phosphates of lead, bismuth, and antimony.
silver phosphate can be reduced and yields finely divided metallic silver and phosphoric acid, which is catalytically reduced in the presence of the
silver to give free phosphorus.
lead phosphate is reduced under hydrogen or methane with hydrogen resulting in the highest yields and methane at 50% The reaction consists of three
stages: 1. The Pb3(PO4)2 is heated up to 300C to drive off any existing water. 2. Once the temp hits 300C the hydrogen is turned on and the
tempurature slowly raised to 500C. The hydrogen reduces the Pb3(PO4)2 by ripping off the oxygen molecules and forming Pb3P2, aka lead phosphide. 3.
Upon the cessation of evolution of water, the furnace is again slowly raised up to somewhere between 650-800C. According to the patent, small amounts
of PH3 are liberated at around 600C. This makes sense, the Pb3P2 probably starts to break down somewhere around 600C and thus liberates PH3, which
subsequently start to be reduced to H2 and elemental P at around 650C, so basically at the beginning of the reduction temp the phosphine being
liberated is not hot enough to break down. phosphates can be reduced by hydrogen at temperatures between 300° and 750°C. Lead phosphates are
particularly easy to reduce by hydrogen. For example, pyromorphite, 3Pb3(PO4)2*PbCl2, starts to react at 300°C and is completely reduced at 850°C.
Other possible reducing agents CaC2 would make a good reducing agent in such a reduction as phosphate reduction. I suspect that sodium polysulfide
would work well in a phosphate reduction. 4Na3PO4 + 2Na2S2 ----> 8Na2O + 4SO2 + P4 Using sodium acetate as a carbon source fusing Hexasodium
metaphosphate with Sodium acetate the mixture liquefies quickly and a strong smell of garlic was released. Sodium acetate acting as a carbon source
and a flux because once the melt was fluid there was a large release of Phosphorus.
Phosphorous from phosphine
phosphine with dimethylchloramine, which reacts to form elemental phosphorus and dimethylammonium chloride (as reported here: http://pubs.acs.org/doi/abs/10.1021/ic50067a009)
C2N14 excerpt of synthysis
by Engager And Tdep
calcium cyanamide
heating a mixture of calcium oxide and urea at 120-350 °C which gives calcium cyanate, followed by calcination at 7-900 °C to give calcium
cyanamide
Aminoguanidine
prepared from calcium cyanamide and hydrazine sulfate. Reaction produces impure aminoguanidine, which is then converted to aminoguanidine bicarbonate
for easier purification
5-AminoTetrazole
through the action of nitrous acid and aminoguanidine
Disodium 5,5'-AzoTetrazole
is produced by the reaction of KMnO4 and 5-AminoTetrazole
Isocyanogen Tetrabromide
Bromine rips apart the tetrazole groups to form an obscure molecular motif, needed to make the famed C2N14 energetic compound
C2N14 (soulble in acetone) The distilled water is added to the isocyanogen tetrabromide this is so the excess bromine is pulled into the water Sodium
thiosulfate is added to nutrilize the bromine The thiosulfate solution above the solid is remove then washed with distilled water then acetone is
added which the isocyanogen tetrabromide redesolved in the acetone This is placed in an ice bath to 0C
sodium azide is desolved in water it is added to the cyanogen tetrabromide acetone solution. The solution is then allowed to return to room
temperature Water is added to precipitate the product. This is then put back into the ice bath to precipitate the crystals. ----
Hydrazine Sulfate
synthesis solution of 10% sodium hypochlorite is added to solid sodium hydroxide and the mixture is kept cold during the addition. Meanwhile, a
solution of urea with a few hundred mg of gelatin is prepared. The two solutions are mixed and allowed to fully react, a voluminous foam will appear.
After they have reacted, MEK is added to the solution and the azine is processed as previously described.
Sodium azide
Isopropyl nitrite reacts with hydrazine hydrate and sodium hydroxide to form sodium azide
Isopropanol nitrite
Concentrated hydrochloric acid is slowly dripped onto sodium nitrite suspended in isopropanol, generating nitrous acid which reacts with the alcohol.
Organic Chemistry
Acetic Anhydride
Many amateurs have attempted to make acetic anhydride at home due to its tremendous usefulness in organic chemistry. Only a few have succeeded,
though a write-up of the preparation of acetic anhydride from sulfur, bromine, and anhydrous sodium acetate was reported by Magpie. Another more
accessible method involves the reaction of acetyl chloride and anhydrous sodium acetate.[1]
A preparation that is as of yet not well-researched involves the dry vacuum distillation of anhydrous zinc acetate, which gives off acetic anhydride
and converts to basic zinc acetate. If achievable, this would mean a route to acetic anhydride that only requires glacial acetic acid and cheap zinc
metal.
Preparation of Acetic Anhydride by Magpie
8CH3OONa + S +3Br2 = 4(CH3O)2O + 6NaBr + Na2SO4
anhydrous sodium acetate and set aside in a covered beaker. Weigh out 3.5g (0.11 moles) of sulfur in a beaker and set aside. Have available 20 mL
(0.39 moles) of dried Br2.
Mix the bromine and sulfur together anhydrous sodium acetate
bromine is the limiting reagent. The sulfur, except that released as SO2, is recycled in situ. Vacuum Distillation Set up for vacuum distillation of
the Ac2O using the 3-neck 500mL RBF. Place an insulating blanket over the RBF. With a vacuum of 23”Hg (absolute pressure = 178 mmHg) the Ac2O comes
over at about 72°C. Yield of the crude Ac2O will be ~30 mL. E. Simple Distillation Set up for simple distillation of the crude Ac2O at atmospheric
pressure. Use a 50 mL RBF as pot. Collect 2 cuts. The first cut (~15 mL) will come over at about 128-135°C. The 2nd cut (~10 mL) will come over at
135-143°C. Literature value for the bp of Ac2O is 140.0 °C. Yield, based on the 10mL of cut 2 and the amount of Br2 charged, is ~27%.
FORUM MATTERS
Ever wonder how many members are in sciencemadness
We have 288131 mad scientist members.
Spam problem eliminated With the change of registration to email only (date start needed) sciencemadness is finally is not having problems with
constant spam alot of hard work was going into avoiding this last resort but the board has benefited from the change. With even a span killer
designated to take on the problem before and a subform named Test Forum with the Forum Moderator as streety It was a Test area for testing spam
prevention mechanisms.
The message everyone sees is the reasoning
The management apologizes for the inconvenience, but it is necessary to keep abusive users and bots out.
PERSONAL DEVELOPMENTS
Tdep's great new (top secret) job doing chemistry for the military.
Metacelsus heading off to the UK to pursue some great opportunities in education.
Cou's business venture of fragrance compounds
LEGAL AND CHEMICAL AVAILABILITY ISSUES
Changes in availability of chemicals / equipment.
#
Changes in legislation that affect members.
#
Recognition of collaberation (subjected to change as more help add)
J_sum1
Heptylene
Cou
clearly_not_atara
Texium (zts16)
References
Make Sulfuric Acid (Copper Sulfate Electrochemical Method)
https://m.youtube.com/watch?v=5dUSF9Gl0xE
Sulfuric acid water and sulfur (electrobromine process)
https://m.youtube.com/watch?v=6ms6xbPhdVs
Make Sulfuric Acid by the Copper Chloride Process
https://m.youtube.com/watch?v=l2AkVYxDSKc&t=13s
Make Sulfuric acid (metabisulfite/oxidizer method)
https://m.youtube.com/watch?v=okvvD3-DF9U
-------
Sulfur trioxide
http://www.sciencemadness.org/smwiki/index.php/Sulfur_trioxi...
Sulfur Trioxide and Oleum, by GARAGE CHEMIST [Publication]
http://www.sciencemadness.org/member_publications/SO3_and_ol...
--------
Ostwald style nitric production [Technochemistry]
http://www.sciencemadness.org/talk/viewthread.php?tid=71282
---------
Preparation of elemental phosphorus [Prepublication/Chemistry in general]
http://www.sciencemadness.org/talk/viewthread.php?tid=65
Preparation of Acetic Anhydride
[Prepublication/Organic chemistry]
http://www.sciencemadness.org/talk/viewthread.php?tid=15021
--------
C2N14 (azidoazide azide)
https://m.youtube.com/watch?v=uNhVK-2mh6w
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Antigua
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I like the idea of a report like that, but there is a ton to change. Most of these excerpts aren't written gramatically correctly and I feel like you
chose to go by "quantity over quality". If one is to call such report "journal-ish", they have to step up their game. I don't want to sound aggresive,
though - keep up the work, it's just there's still a lot of it to do.
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symboom
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You don't sound aggressive you are stating your opinion. Most of the excerps are just copy and paste I am greatful for feed back. I will go back and
work on what I have so far and improve the quality. I'm more aiming for newsletter format like this is what has gone on in amature chemistry.
Oh I copy and pasted the older version damn well at least everyone can see the progress
Maybe I need to take a look at how newsletters look and how it's worded along with the information of how the procedures are done.
sorry about the bad format when i copy and past it removes my formating
____________
Nitric acid from ammonia Oswalt style (without platnium)
This process uses urea as a source of ammonia which is heated till it decomposes into ammonia and carbon dioxide, oxygen is added to the system using
an Air compressor. A condenser is used to dry the ammonia/air stream. The ammonia air mixture is fed into a Quartz tube with a 8mm ID that is heated
with nichrome wire heating element. The reaction chamber contains NiO or CoO as a Catalysis that are supported bed of Sand or a red brick chunks. The
ammonia is oxidized to nitrogen monoxide. The Quartz tube runs into an Absorption tower (converted 2L sep. funnel water with broken glass to increase
surface area. which admits air via the custom condenser fitting. The absorption tower oxidizes the nitrogen monoxide to nitrogen dioxide which
combines with the moisture of the reaction to produce nitric acid.This condensate runs into a reservoir to collect the Nitric acid the excess gasses
run to a vertical anti suck back column before running along a small tube to the base of the tower.
____________
Sulfur trioxide
The preparation of Sulfur Trioxide is extremely dangerous and should only be attempted by chemists with experience working with hazardous volatile
reagents.
Pyrolysis of Sodium bisulfate first evolves water, forming sodium pyrosulfate, which then decomposes above 460 °C to sodium sulfate, releasing Sulfur
Trioxide this reaction temperature can be lowered to 150°C if concentrated sulfuric acid is added to the Sodium Bisulfate.
Pyrolysis of transition metal sulfates can also be used to make sulfur trioxide. Heating iron(III) sulfate at 480 °C it decomposes produces mostly
sulfur trioxide. Heating copper(II) sulfate above 560 °C yields sulfur trioxide. Heating iron(II) sulfate at 700 °C with carbon yields iron(III)
oxide, sulfur dioxide and sulfur trioxide. Aluminium sulfate also works, though the decomposition temperature is slightly higher.
Roasting calcium sulfate with silicon dioxide (very fine sand can be used) at 1000 °C for 1 hour yields calcium silicate and sulfur trioxide. Adding
small amounts of chromium(III) oxide or tungsten(IV) oxide improves the process.
Sulfur trioxide can also be obtained by oxidizing sulfur dioxide in the presence of several metal oxides, such as copper(II) oxide at high
temperatures or chromium(III) oxide (at 180-400 °C).
Adding phosphorus pentoxide to extremely concentrated sulfuric acid will release sulfur trioxide, which can be extracted via distillation.
Metaphosphoric acid can also be used instead of the pentoxide.
[Edited on 25-10-2020 by symboom]
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Herr Haber
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Just a thought... if there's a feeling that you're going for quantity over quality is probably just means that you have material for not just one but
two issues of the journal.
Having it neatly organized over time might be very interesting as a reference book.
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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symboom
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I need to format this better to constrain it to look like a newsletter for it to be about like this is what going on in amature chemistry.
I read a lot of journals so i think I have that format stuck in my mind.
My goal is that it can inspire others to get involved in the community whether it's the wiki, writing the book for chemistry, The newsletter, finding
research to synthysis and properties of compounds and performing experiments. It takes a long time to compile the information from Threads and look up
articles. I've seen some prepublications that have done this.
[Edited on 26-10-2020 by symboom]
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clearly_not_atara
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We want typesetting!
I'll try to mock something up this weekend if nobody gets to it before me.
[Edited on 04-20-1969 by clearly_not_atara]
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symboom
International Hazard
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http://www.sciencemadness.org/talk/files.php?pid=648083&...
He is an update it's a .doc file
[Edited on 3-11-2020 by symboom]
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Antigua
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Looking much better! I've only got a couple of comments.
1. Should we really consider things like carbon, charcoal and silicon grease important chemical reagents? When was the last time You guys used
charcoal (not as a decolorifier) or chucked a tube of grease into the reaction flask? That's being picky, I know, but doesn't sit right with me if
this journal is supposed to be 100% accurate.
2. You should definietly employ index numbers while writing chemical formulas, Pb2O3 does not look professional.
3. A lot of interpunction needs to be fixed
Other than that it's a pretty decent overview/abstract on what this forum is about.
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symboom
International Hazard
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here is the updated file with the improvements stated
Thank you Antigua for the feedback
Attachment: mad science report2.doc (83kB)
This file has been downloaded 363 times
[Edited on 6-11-2020 by symboom]
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