Nuclear and High Voltage Science

N U C L E A R A N D H I G H V O LTA G E S C I E N C E
Vacuum System For

The Fume Hood
Don’t mind the mess…
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Put together a much needed vacuum system for my fume hood
entirely out of spare parts I had lying around. The pump,
pressure switch and gauge actually came from a professional
vacuum apparatus but I took it apart to repurpose it for myself, it
also had a little compressor which I may or may not make use of
at some point. The tank is from a pressure equalizer and
everything else is just stuff I already had.
The construction is pretty simple and self explanatory. I added a
trap full of indicating silica gel to remove moisture, there will
also be an overflow trap between the outlet and whatever I am
using it on. If I wish to vacuum distill any acids then I will just
add a bubbler with saturated NaOH.
In my original design the valve and gauge were going to be in
different spots so thats why I ran two hoses but I wasn’t really
thinking about that after I changed it. I should have just put a tee
on the main line, it’s purely asthetic though…
In all the system works really well and I didn’t have to bother
with finding leaks so that was nice. The pump goes down to
400mBar and shuts off, it kicks back on at 500mBar.
March 27, 2023 General Chemistry
acid, chemistry, distillation, fume, hood, pressure, pump, science, system, uranium,
vacuum
Simple methods for
producing various
uranium compounds
I dont currently have a big stock of uranium so many of these are low volume or dilute.
My main interest in uranium chemistry for a while was just to

refine some metal but as I have grown more advanced in
chemistry it has shifted to the unending number of amazing
compounds it makes. I try to stay relatively low budget so here I
will discuss methods for producing them in a home lab and I will
continue updating this as I discover new ones. In most cases
uranyl nitrate will be the starting compound.
OXIDES
URANIUM DIOXIDE
The simplest method I’ve come across to make UO2 is to

decompose uranyl oxalate.
UO2(NO3)2 + C2H2O4 = UO2C2O4 + 2HNO3
Boil the solution to drive off the HNO3, continuing heating will
remove waters of hydration, CO2 and then decompose to UO2 in
an inert atmosphere or UO3 in the presence of oxygen. A

blowtorch or kiln is needed to reach the necessary temperatures,
although I don’t have the exact number, above red hot is a good
target. Heating in a tube or container with loose lid will cause it
to fill with CO2 from the decomposition and yield pure UO2.
URANIUM TRIOXIDE & TRIURANIUM OCTOXIDE
UO3 can be obtained by heating many uranium compounds to

decomposition including ammonium, nitrate, and peroxide.
Complete decomposition temperatures and time varies but a few
minutes at 300C should get you there and you will end up with a
bright orange powder. If you notice it turning dark green then
you’ve applied too much heat and converted it to U3O8 which
occurs around 700C.
URANIUM PEROXIDE
Uranyl peroxide is as simple as adding concentrated H2O2 (~30%)

to a solution of UN in nitric acid. Much more information on this
process can be found here.
https://www.911metallurgist.com/uranium-precipitation-
hydrogen-peroxide/
UO2(NO3)2 + H2O2 = UO4 + H2O + HNO3
ALKALI SALTS
DIURANATES
Alkali diuranates are made by neutralizing UN with an alkali

hydroxide giving the diuranate (MxU2O7) Where M is the alkali
and x is the quantity. In the case of magnesium, MgO is used
which hydrolyzes to Mg(OH)2 in solution.
Examples: ammonium (NH4)2U2O7, sodium Na2U2O7, magnesium

MgU2O7
URANATES
Uranates are created by combining oxides at high temperatures

or thermal decomposition of salts. Eg: Na2O + UO3 → Na2UO4. I
have not made any uranates yet so I don’t have much to say
here…
Image borrowed from wikipedia
https://en.wikipedia.org/wiki/Uranate
FLUORIDES
URANIUM TETRAFLUORIDE
UF4 is made by reducing UO2Cl2 to UCl4 and reacting with HF.

UO2Cl2 is made by reacting any U oxide with HCl. Two good
reducers are Zn and Sn dichloride. I have another blog describing
how I made a PTFE apparatus for making HF.
UO2Cl2 + SnCl2 + 4HCl = UCl4 + SnCl4 + H2O
UCl4 + 4HF = UF4 + 4HCl
URANIUM HEXAFLUORIDE
Most of the routes to UF6 involve reaction with fluorine gas

which is beyond the scope of any home lab and most professional
ones but there is one route that is relatively simple. On the right
side of the picture below there is a route that uses the thermal
decomposition of UF4 to UO2F2 and UF6. This method is not used
in industry due the formation of byproducts and thus there is
very little information about it. I have not yet attempted it but I
believe a copper reactor with a tube going into a glass vial
containing NaF or KF in dry ice would work well. Alkali fluorides
are effective desiccants for UF6, without them, any water present
in the UF6 would destroy the glass by a cyclic reaction creating
HF and more water.
CHLORIDES
There exists 5 chloride species of U. III, IV, V, VI, and UO2Cl2.

UO2CL2 and UCl4 were discussed in the synthesis of UF4 so I
won’t go into them here.
URANIUM (III, V, VI) CHLORIDE
UCl3 can be made by reacting UCl4 with hydrogen at high

temperatures, UCl5 can be made by reacting UCl4 with Cl at 550C
and and UCl6 is made by blowing Cl gas over sublimated UCl4.
UNCATEGORIZED
URANYL SULFATE
UOx + H2SO4 = UO2SO4

October 21, 2022 General Chemistry
acid, aqueous, chemistry, chloride, fluoride, fluorine, H2SO4, hexafluoride, hydrogen,

nitrate, nuclear, organic, oxidation, oxide, peroxide, PTFE, purex, science, sulfuric,
tetrafluoride, trioxide, uranium, uranyl, urex
Building a fumehood
for home chemistry
Before getting into nuclear chemistry I always just did all my
experiments in the kitchen and even for a while of doing
uranium chemistry I was still doing it in the kitchen and for very
obvious reasons I couldn’t keep doing this. The design I have
come up with here is very simple and easy to build with some
basic skills and only cost about $200. I am doing going to go into
specifics of each part was assembled, rather this is meant to be a
guide so basic building and design skills are necessary.
MATERIALS
– 2 sheets of 3/4″ 4×8 MDF (one of them cut in half longways)
– 2 sheets of 3/4″ 2×4 MDF
– 6 8′ 2×4
– 2 sheets of 1/4″ 2×4 MDF
– Lots of screws, 2.5″ and 1.25″ mostly
– A sheet of glass or plexiglass big enough to cover most of the

opening
I started by building a frame for the work surface. I measured the

height of a table to get a feel for how high it should be and after a
couple years of use I am happy with what I’ve got. You will notice
that the horizontal dimension is 49″, this is what the length of the
2×4 and width of the 4×8 MDF boards were. Not sure why they
aren’t 48″.
All the pieces laid out
I know my drawing is pretty crude but it works!
Next I added the sides. They are simply screwed to the legs on the
table and then I added the top frame. You will see that the side
pieces of the top are recessed a little, this is so I can add a piece of
trim and it will sit flush with the sides. The height of the top was
determined by the size of the plexiglass screen that I had which
came from a TV.
I didn’t think about this during construction but the blower must be mounted at the window and not at
the unit! I eventually replaced this plastic sash with a piece of tempered glass.
Next I painted the inside. I used ourdoor acrylic deck paint, it has
proven to be pretty tough and holds up well. Because there is no
overlap at the corners I used silicone to seal them inside and out.
Apply this before painting.
After multiple coats of paint I added a light and a baffle with one
of the 1/4″ MDF boards to help even out the exhaust flow and
force air to be pulled to the back of the hood. I only left a small
gap at the top so that most of the air flows through the bottom.
Also some trim was added to the sides for the sash to be screwed
to.
Testing the fit
The square hole on the top was made round and a PVC toilet
flange was used to attach 4″ vinyl duct. Another toilet flange was
screwed and sealed with silicone to the blower inlet. I built a
mount for the window which allows me to remove the blower.
Because I have double windows the outside of the outer board
was painted and a flap was added to close the hole when the
blower is not in.
This Chinese adjustable hole saw is a little scary but has proven to be a valuable tool.
Next I painted the baffle and added the rack using 1/2 Al rods that
I bought on eBay, I already had the mounts. I finished up with the
trim and secured the sash. The trim on the sides was cut short so
that the other 1/4 MDF board could be slid in and out as a
removable work surface. I use appliance epoxy spray paint to
protect it although it doesnt stand up well against harsh
chemicals, it still lasts for a long time if you take care of it.
Testing out the blower while I was waiting on my vinyl duct to arrive.
After getting my lab put together and a year of us it inevitably gathered lots of clutter.
acid, aqueous, chemistry, distillation, fume, hood, organic, science
PTFE apparatus for

producing
hydrofluoric acid
The finished setup, ready to distill.
This is a very short and simple explanation of how I built an

apparatus for producing HF which I needed to make UF4 in my
quest to refine uranium from ore. Obviously HF is incredibly
dangerous so I can’t be responsible for anything you do with this
information.
I got a 200ml PTFE reaction vessel on amazon, it is a perfect

choice for this application. I used 10x12mm (ID, OD) tubing and
drilled a hole 10.8mm (7/16 or something like that?) into the side
of the vessel and heated the tubing to force it into the hole. After
heating again the tube expands to its original size and makes a
very tight seal. The same thing was done to attach the condenser
since adhesives & sealants aren’t much of an option for PTFE. The
condenser is just a 3/4″ PVC tube with hose barbs and caps on
either end. The reactor was wrapped tightly in copper wire to
distribute the heat evenly and is placed in a sand bath. The
receiving flask is PP with a tightly sealing lid which is charged
with water prior to running so it converts directly to HF acid.
I did my first test run with 50g of CaF2 and 90ml of H2SO4. I only
got about 50% yield, the rest was still in the reactor but after 3
hours I finally shut it down. The evolution of HF is very slow. I
added ice to the remaining sludge to cool and dilute it, it makes
an excellent rust cleaner!
If one wishes to make HF just know that the CaF2 and H2SO4
mixture will foam up a lot. Start small and keep your total
volume of reactants to less than half the volume of the container.
acid, aqueous, calcium, chemistry, distillation, fluoride, fluorine, gluconate, H2SO4,

hydrogen, nuclear, PTFE, science, sulfuric, teflon
Recovering pure
uranyl nitrate with
tributyl phosphate
Waste solution next to TBP after extraction
Here I will describe my experience with using TBP to obtain very

pure UO2(NO3)2. There are only a few scenarios where I see this
being useful in the realm of hobby chemistry because it is fairly
easy to get pretty pure uranium from the standard processes
using acid or carbonate leach.
Two such scenarios are:
– Recovering U from small amounts of high grade ore
– Recovering U from samples with unknown contaminates
PROCESS
This only requires 5 ingredients and some glassware that any lab
should be stocked with.
– Compound to be extracted
– 5M Nitric acid
– TBP
– Kerosene
– Water
For glassware you will need a stoppered flask and a seperatory

funnel large enough to contain the entirety of the aqueous and
organic solutions. A stir plate helps but is not necessary. As for
TBP, I got mine from a friend who is a professional chemist, the
only cheap source I’ve found online is alibaba. I was quoted $80
for 1kg of TBP with shipping, might be able to get a better deal
from other sellers though.
Start making a mixture of 30% TBP in kerosene. I use 1-K from

ace hardware, it’s pretty clean and cheap. Dissolve the uranium
compounds in the nitric acid, this may require heating. It takes 2
mols of TBP per 1 mol of U so keep this in mind as to not saturate
the organic phase, if you dont know how much uranium is
present then best to err on the low side. If there is any
undissolved particles at all then it must be filtered as they will
create an emulsion. If you are extracting straight from ore then
then you must remove the silica which can be done by
simmering the solution with gelatin which will polymerize with
the silica. A centrifuge would be a good option to remove the gel
but I suppose a filter would work too, I haven’t tried doing this
yet so I can’t provide much details here. If you do run into an
emulsion, add small amounts of acetone and stir gently until it
disappears.
On my first attempt I had undissolved solids in the solution which I did not know would cause this. The
emulsion got much worse than pictured.
Add your nitrate solution to the TBP solution in a closed flask and
mix vigorously. You will see the yellow uranium nitrate go into
the upper organic layer, I allow a few hours of contact time for
this, best to leave on a stir plate at this stage. After a while you
will notice that the TBP does not get any darker and at this point
it is ready to be separated and then recovered from the TBP.
UO2(NO3)2 after migrating into TBP
Add the mixture to the seperatory funnel and drain off the
aqueous layer. The best thing I’ve found to recover the uranyl
nitrate is near boiling water, sodium bicarbonate solution works
really well but then you end up with sodium contamination in
your product. Multiple washes are necessary as well as multiple
extractions on the starting product to get a full recovery. Be
careful when adding the hot water as the TBP mixture will
ecaporate and build pressure fast in a sealed vessel. I prefer to
use the same flask as before but loosely stoppered.
UO2(NO3)2 is very fluorescent and you can gauge how much is dissolved.
Once you have your uranium nitrate back into water you can add
hydrogen peroxide or ammonia to precipitate either uranium
peroxide or ammonium diurinate and filter it. Both of these will
convert to UO3 upon strong heating, around 300C. Stronger
heating will result in U3O8. Either oxide makes a good form to
store your uranium stock in, as is done in industry.
However… the precipitates of adding H2O2 or NH3 to the

solution are incredibly fine and hold on to a lot of water and
even small amounts will take a long time to dry even at high
temperature. You will loose a small amount through the filter and
also a lot will stick the filter which is not easy to scrape off, it is
the consistency of peanut butter. If you wish to avoid this extra
work you can just boil down the nitrate solution which will also
decompose to UO3.
Small jar of UO3 recovered from TBP
Due to the difficulty of back extraction into the aqueous phase I

started looking for a better method and I found oxalic acid to be
quite effective. I made an arbitrary concentration by dissolving
1g in 15ml of water and heating to near boiling, it effectively
clears the TBP on the first wash. It cannot be precipitated with
ammonia like UN but it can be boiled down and decomposed to
UO2 if no O2 is present or UO3 with O2.
Testing my new method. The water in the flask was as attempt to recover the UN from TBP but it didn’t
want to go into it. The test tube contains oxalic acid and it went into the water no problem, the TPB still
looks yellow from reflection of the flask.
October 6, 2022 Nuclear Chemistry
aqueous, chemistry, crud, emulsion, extraction, kerosene, nitrate, nuclear, organic,

oxide, peroxide, phosphate, purex, science, solvent, tributyl, trioxide, uranium,
uranyl, urex
A site for me to document and share my projects with other

home scientists.
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N U C L E A R A N D H I G H V O LTA G E S C I E N C E

Vacuum System For

Don’t mind the mess…

My main interest in uranium chemistry for a while was just to

The simplest method I’ve come across to make UO2 is to

UO2(NO3)2 + C2H2O4 = UO2C2O4 + 2HNO3

an inert atmosphere or UO3 in the presence of oxygen. A

URANIUM TRIOXIDE & TRIURANIUM OCTOXIDE

UO3 can be obtained by heating many uranium compounds to

Uranyl peroxide is as simple as adding concentrated H2O2 (~30%)

UO2(NO3)2 + H2O2 = UO4 + H2O + HNO3

Alkali diuranates are made by neutralizing UN with an alkali

Examples: ammonium (NH4)2U2O7, sodium Na2U2O7, magnesium

Uranates are created by combining oxides at high temperatures

UF4 is made by reducing UO2Cl2 to UCl4 and reacting with HF.

UO2Cl2 + SnCl2 + 4HCl = UCl4 + SnCl4 + H2O

UCl4 + 4HF = UF4 + 4HCl

Most of the routes to UF6 involve reaction with fluorine gas

There exists 5 chloride species of U. III, IV, V, VI, and UO2Cl2.

URANIUM (III, V, VI) CHLORIDE

UCl3 can be made by reacting UCl4 with hydrogen at high

UOx + H2SO4 = UO2SO4

acid, aqueous, chemistry, chloride, fluoride, fluorine, H2SO4, hexafluoride, hydrogen,

– 2 sheets of 3/4″ 4×8 MDF (one of them cut in half longways)

– 2 sheets of 3/4″ 2×4 MDF

– A sheet of glass or plexiglass big enough to cover most of the

I started by building a frame for the work surface. I measured the

Testing the fit

acid, aqueous, chemistry, distillation, fume, hood, organic, science

PTFE apparatus for

This is a very short and simple explanation of how I built an

I got a 200ml PTFE reaction vessel on amazon, it is a perfect

acid, aqueous, calcium, chemistry, distillation, fluoride, fluorine, gluconate, H2SO4,

Here I will describe my experience with using TBP to obtain very

Two such scenarios are:

– Recovering U from small amounts of high grade ore

– Recovering U from samples with unknown contaminates

For glassware you will need a stoppered flask and a seperatory

Start making a mixture of 30% TBP in kerosene. I use 1-K from

However… the precipitates of adding H2O2 or NH3 to the

Due to the difficulty of back extraction into the aqueous phase I

October 6, 2022 Nuclear Chemistry

aqueous, chemistry, crud, emulsion, extraction, kerosene, nitrate, nuclear, organic,

A site for me to document and share my projects with other

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