Homemade Smokeless Powder

Albert9x19

Alpha documentation
Current as of 19th Aug 2022

Preface:
Making homemade smokeless powder involves using dangerous chemicals to produce
dangerous & potentially dangerous products. If you choose to attempt this, you are responsible
for your safety & actions. This guide should be read in its entirety first & then followed very
closely. If you are still unsure you can message me on Key base or Rocket Chat at Albert9x19,
look to the information folder, or do your own research as to the methods & safety surrounding
this project.

What is smokeless powder?

Smokeless powder is nitrocellulose. Nitrocellulose (NC) is nitrated cellulose; cellulose is
commonly found as the make-up of paper or cotton. The nitrating solution is an equimolar
mixture of sulfuric acid (H2SO4) & nitric acid (HNO3) Equimolar meaning equal moles of
solution, sulfuric acid (H2SO4) is 98 grams per mol & nitric acid (HNO3) is 63 grams per mole.
An equimolar solution would have 63 grams of HNO3 mixed with 98 grams on H2SO4.

Smokeless powder can often be used in firearms as either a single base powder or a
double base powder. Singe base powders burn slower & often are used in rifle rounds & only
contain NC. Double base powders are a mixture of NC & nitroglycerin (NG). There are triple
base powders but those will not be discussed as they are not commonly used for small arms.

This project will continue to evolve expanding to more methods of acid procurement,
process improvement, & load data.

Definitions:

Ice bath – a container containing cold water & ice. Example: a small, shallow glass baking dish
can be used as the container; it is filled one quarter of halfway with cold water & ice is added.
This is used to chill acids throughout the process. It is important not to over fill the container as;
one, it may over flow when the beakers are placed in & two, small beakers containing small
quantities of acids may float & tip over spilling into the ice water.

Tare – to zero out the scale.

Procedures:

Weighing out chemicals – To properly weigh out chemicals the place the scale on a flat hard
surface, turn on the scale, place the beaker in which chemicals are to be measured in on the scale,
the scale should now have a reading, the units should be changed to grams (g), the “zero” or
“tare” button is pressed to zero out the scale. Upon reading zero, chemicals can be weighed out.
Units listed throughout this document are given in grams. Liquid chemicals should not be
measured in ml as 100 ml of water weighs less than 100 ml of sulfuric acid due to the different
densities of the liquids. For example water weighs 1 gram per milliliter (ml). Meaning 100 ml of
water will weigh 100 g. Sulfuric acid weighs 1.83 grams per milliliter (g/ml) meaning 100 ml of
sulfuric acid will weigh 183 grams.

Acid Procurement:

The two acids required are sulfuric acid (H2SO4) & nitric acid (HNO3). Ideally, we
would like 98% H2SO4 & 68% HNO3 & that will be the focus although other methods will be
developed in the future such as using just drain opener & KNO3, no distillation required, this is
crude but works.

H2SO4:

A simple source of H2SO4 is found in drain opener. Some drain openers are 98% H2SO4
with inhibitors added, while others contain sodium hydroxide & cannot be used so it is important
to read the contents of the bottle. It is then distilled to yield clean H2SO4. Alternatively, it can be
derived from copper sulfate, which is commonly found as a root killer, used in aquariums & used
in homebrewing of beer/seltzer/wine. It will come either as a crystal or liquid. The crystal is
dissolved in water & electrolysis is performed. This results in dilute H2SO4 which is then
purified via distillation. As other methods of acid derivation are explored this document will be
updated to include them.

HNO3:

The primary derivation of HNO3 is reacting potassium nitrate (KNO3) with H2SHO4 to
produce HNO3 & potassium bisulfate (KHSO4). This is then distilled. KNO3 is often sold as a
stump remover in the lawn & garden section. The other derivation is through the use of a
Birkland-Elyd reactor where nitrogen dioxide (NO2) is produced, bubbled through water & then
distilled. This method is far more time consuming & is not energy efficient but works & can be
done if KNO3 cannot be procured. Friend & fellow enthusiast Cathode G has plans for a
Birkland-Elyde reactor which will be included in this folder with its own instruction for
operation. The distillation process will be the same. As other methods of acid derivation are
explored this document will be updated to include them such as the use of instant cold packs
containing ammonium nitrate. HNO3 can be made using ammonium nitrate & sulfuric acid.

Acid Distillations: The heat setting on the heating mantle does not need to be all the way up,
medium to medium-high will suffice.

H2SO4 Distillation:

*Note* when working with acids the following PPE must be worn; goggle/wrap-around eye
protection, long selves, long pants, gloves, & tie back long hair.

*First aid: Please see the SDS sheets in the additional materials folder
H2SO4:

Inhalation: Move victim to fresh air. Keep at rest in a position comfortable for breathing. If
breathing is difficult, trained personnel should administer emergency oxygen. DO NOT allow
victim to move about unnecessarily. Symptoms of pulmonary edema may be delayed.
Immediately call a Poison Centre or doctor. Treatment is urgently required. Transport to a
hospital.

Eye contact: Quickly and gently blot or brush chemical off the face. Immediately flush the
contaminated eye(s) with lukewarm, gently flowing water for at least 30 minutes, while holding
the eyelid(s) open. If a contact lens is present, DO NOT delay flushing or attempt to remove the
lens. Neutral saline solution may be used as soon as it is available. DO NOT INTERRUPT
FLUSHING. If necessary, continue flushing during transport to hospital. Take care not to rinse
contaminated water into the unaffected eye or onto the face. Immediately call a Poison Centre or
doctor. Treatment is urgently required. Transport to a hospital.

Skin Contact: Quickly take off contaminated clothing, shoes and leather goods (e.g. watchbands,
belts). Quickly and gently blot or brush away excess chemical. Immediately flush with
lukewarm, gently flowing water for at least 30 minutes. DO NOT INTERRUPT FLUSHING. If
it can be done safely, continue flushing during transport to hospital. Immediately call a Poison
Centre or doctor. Treatment is urgently required. Transport to a hospital.
*Pulmonary edema is a condition caused by too much fluid in the lungs. This fluid
collects in the many air sacs in the lungs, making it difficult to breathe. This can result in a what
is referred to as “dry-land-drowning”

Ingestion: Have victim rinse mouth with water. If vomiting occurs naturally, have victim lean
forward to reduce risk of aspiration. Have victim rinse mouth with water again. Immediately call
a Poison Centre or doctor. Treatment is urgently required. Transport to a hospital.

HNO3
Inhalation: If nitric acid mist or vapors are inhaled, immediately move to get fresh air.

Eye contact: Using eyewash, flush eyes while holding eyelids open.

Skin Contact: Flush skin with tepid water for 15 minutes using the closest available sink,
portable drench hose or safety shower. Remove any exposed clothing as well as any jewelry that
may be trapping nitric acid.

Ingestion: Do not induce vomiting

KHSO4

Inhalation: Fresh air, rest. Seek medical attention if you feel unwell.

Eye contact: First rinse with plenty of water for several minutes (remove contact lenses if easily
possible), then refer for medical attention.
Skin Contact: First rinse with plenty of water for at least 15 minutes, then remove contaminated
clothes and rinse again. Refer for medical attention if skin irritation occurs.

Ingestion: Do NOT induce vomiting. Refer immediately for medical attention.

Copper Sulfate:

Inhalation: Remove the victim into fresh air. Respiratory problems: consult a doctor/medical
service. Assure fresh air breathing. Allow the victim to rest.

Eye contact: Rinse immediately with plenty of water. Do not apply neutralizing agents. Take
victim to an ophthalmologist if irritation persists. Rinse immediately with plenty of water. Obtain
medical attention if pain, blinking or redness persist.

Skin Contact: Wash immediately with lots of water. Do not apply (chemical) neutralizing agents.
Take victim to a doctor if irritation persists. Remove affected clothing and wash all exposed skin
area with mild soap and water, followed by warm water rinse.

Ingestion: Rinse mouth with water. Immediately after ingestion: give lots of water to drink. Call
Poison Information Centre (www.big.be/antigif.htm). Consult a doctor/medical service if you
feel unwell. Ingestion of large quantities: immediately to hospital. Rinse mouth. Do NOT induce
vomiting. Obtain emergency medical attention. Immediately call a POISON CENTER or
doctor/physician.

*Note* all distillation of acids should be done outdoors/in a well-ventilated area as to not expose
the operator to the fumes produce which are harmful.

The following distillation is using a 500 ml round bottom flask. Larger or smaller can be scaled
accordingly.

H2SO4 Drain Opener Distillation: The heating mantle is set up & plugged in, the 500 ml round
bottom flask is placed in the heating mantle, a few boiling chips/boiling stones are added (these
will need to be either glass or porcelain as to not react with H2SO4) or they can be made by
breaking up small pieces of glass. A funnel is used to fill the round bottom no more than half full
of drain opener. For 500 ml flask I add 200 ml. If more is added & it starts bumping1, there is the
risk of contaminating the distillate or worse, breaking the round bottom flask. The distillation
apparatus is set up as shown in figure 1 & the neck of the flask & 70o elbow are insulated with
foil. H2SO4 is added to the round bottom flask, the 70o elbow is placed on. The ring stand &
clamp are attached clamp around condenser with the distillate end sloped toward the collection
vessel (this end is usually slanted). The condenser is inserted into the 70o elbow. The 105o elbow
is then added to the distillate end. For H2SO4 distillation metal keck clips must be used, &
plastic must not be used. The flask & neck are insulated with foil as shown. A beaker/glass
container is placed below discharge end. Cooling water is not required for this distillation, so the
condenser tubing (although pictured) & the pump are not required.
 Figure 1

I begin heating the drain opener. At first the color will change & eventually the distillate
will be begin collecting in the beaker below. It typically took just over an hour of heating to
begin seeing distillate, longer when distillation is performed in freezing temperatures. Watch the
videos regarding this distillation in the videos folder for more information. The distillate is
collected watched for a change in density, one will see when the more dense, purer H2SO4 is
being carried over by the way the light refracts through the distillate. This is demonstration in the
video (H2SO4 Density Change). Begin watching more carefully as the density on the distillate
begins to change & occasionally test a drop on a paper towel. Please see my video regarding this
for clarification (H2SO4 test). It will be ready for collection when the acid eats the paper towel
very quicky turning more black than yellow/brown at first. It is better to under collect than over
collect & have weaker acid. Note: Once cooled to room temperature, concentrated sulfuric acid
is very viscous. End Note.
Once confident that the acid is ready to be collected, the collection beakers are swapped,
& the dilute acid is added to a bottle labeled ‘Dilute H2SO4”. I will typically add this into
another batch or run it as its own batch but will dispose of the dilute acid collected from that. If
bumping occurs, turn off the heat & let the unit completely cool, add more boiling stones &
resume heating on a slightly lower heat setting, if the dilute acid has been removed this step of
collecting & testing to see how strong it is does not need to be performed a second time. It is
important watch the level in the boiling flask & ensure that it done not run dry, doing so could
damage equipment or crack the glass. A good stopping point is when the circle of liquid in the
bottom of the 500 ml round bottom flask is about 1.5 inches in diameter or 3.5 cm do not let it
get smaller than that of a bottle cap. Upon turning off the heating mantle, I recommend using a
heat protectant glove to raise the flask removing it from the heating mantle which will remain hot
for some time.
1: Bumping occurs when liquids are heated, or has its pressure reduced very rapidly, typically in smooth, clean glass flasks. As the liquid's
temperature rises above its boiling point, it becomes superheated. Once a bubble has formed, it will grow quickly, turning into a large vapor
bubble that rises, pushing the liquid out of the test tube, typically at high speed. This rapid expulsion of boiling liquid poses a serious hazard to
others & oneself in the lab. (http://www.sciencemadness.org/smwiki/index.php/Bumping)

H2SO4 via copper sulfate:

This process should be done outdoors in a well-ventilated area for safety. To make
H2SO4 using copper sulfate, the required tools & materials include; water, (This does not have
to be deionized/distilled water) copper sulfate, (sometimes listed on the label as copper sulfate
pentahydrate) a battery or power supply, (the one used to ECM barrels will suffice) a copper
electrode (attached to the negative lead) (A piece of copper pipe, rod, or solid wire will suffice),
A platinum (Pt) coated titanium electrode (connected to positive lead of the power supply or
battery) or in place of the Pt electrode a carbon electrode (note this will make the solution dirty
as the carbon electrode erodes, the solution will need to be filtered prior to distillation or, what I
found to work the best, a lead electrode, I just used a chunk of lead from the sprue plate, a
byproduct of casting bullets. Any of the three will work & they should be attached to the positive
lead. A way to connect the anode & cathode to the to the battery or power supply *Note, if
copper alligator clips are used, when connected to the positive lead ensure the clip does not make
contact in the solution as the copper will be eroded*. Please see the shopping list for
recommended tools for this set up. A glass beaker or jar to perform the electrolysis in will also
be required.
Copper sulfate has a solubility of 21g per 100 ml of water at 25C. Meaning that there will
be a saturated solution when 21 grams of copper sulfate are added to 100 ml of 25C water.
Saturated solution meaning that no more copper sulfate can be dissolved into the water. As the
water temperature increases the solubility increases. At 100C 74 grams of copper sulfate can be
dissolved in solution. Preparation of solution entails using warm water & dissolving 25 grams of
coper sulfate per 100 ml. Each batch can be as large as the users would like but a the larger the
batch the longer it will take to react. Typically, I would fill a 1000 ml beaker with 500 ml of
warm water & add in 200 grams of copper sulfate. Figure 2 below displays a 500 ml beaker with
40g of copper sulfate, this was taken while I was still testing this method.
Figure 2
 The solution is a milky-blue color when the copper sulfate is added. The mixture is
stirred thoroughly to ensure all the copper sulfate is dissolved into solution. If most but not all
dissolves into solution this is okay, as the reaction progressed the solution will heat up & it will
be dissolved, or the solution can be stirred. Figure 3 below shows the blue solution upon
dissolving the copper sulfate. It can be various shades of blue depending on how much copper
sulfate is dissolved.
Figure 3
 The negative terminal of the power supply is connected to the copper wire, pipe, or rod &
placed in solution & the positive terminal is connected to the Pt coated titanium electrode, carbon
rod or piece of lead. Figure 3 above shows this with the Pt electrode & a piece of copper wire
while figure 4 below shows a piece of copper pipe & lead. Please note that Figure 4 below
depicts the solution mid reaction.
Figure 4
 With the solution mixed in a glass beaker or jar, the anode & cathode in solution making
sure they are not touching, & the leads from the power supply or battery connected, the power
supply can be turned on or the wires connected to the battery. The positive electrode will begin
bubbling, this is hydrogen gas, keep away from open flames & do not inhale. As the reaction
progresses, if using a lead electrode, the solution will begin to turn from blue to clear. If using
the Pt electrode, I found that the solution would begin to turn green. I have not tried the carbon
rods, but they will erode & turn the solution black from the carbon erosion. If the solution turns
black the reaction should be stopped & the solution filtered. Upon filtering the reaction can
resume so that the color change from blue to clear can be observed. *This is why I found the lead
electrode to work best, it did not erode nor did the solution turn green or black (the green color
will stay, the black carbon can be filtered out) *. Figure 5 below shows the set up for the
reaction. Note: the reacting solution is beginning to turn clear (Left) & there is another beaker on
the right mixed & ready to react upon completion of the solution on the left. The dark solution in
the back on the right was reacted using the Pt electrode.
Figure 5

As the reaction progresses copper can be observed falling out of solution depositing on
the copper rod, the copper rod or wire does not need to be cleaned of the spongey copper unless
it is contacting the positive electrode. Figure 6 below shows the spongy copper depositing on the
copper pipe.
 Figure 6

Figure 7 below is another depiction mid reaction of the solution turning blue to clear & the
copper depositing onto the copper rod. Note: the positive copper alligator clip connected to the
lead electrode is touching the solution, as stated above this is to be avoided as this clip was
eroded away & needed to be replaced.
Figure 7

If a variable power supply is used, there is no ideal amperage setting unlike the ECM process,
but the variable power supply is preferred over a battery as the voltage/amps should be
controlled such that the solution does not begin to boil.
As the solution becomes clearer it may be observed that the solution is lightly tinted blue
& the copper rod is beginning to bubble. The reaction can be stopped at this point. The reaction
can progress until the solution is completely clear, but this is very time consuming & most of the
copper sulfate has been reacted, I found it was not worth the time & ended the reaction. Another
observation may be one in which the solution is blue near the bottom of the beaker & clear near
the top, the solution can be stirred continue until it is all clear or evenly slightly tinted blue.
Figure 8 below shows where both the copper & the lead electrode are bubbling.
 Figure 8

It is difficult to see but both are bubbling, & the solution is a milky white. In the videos folder
there is a video titled “Video TITLE” showing the copper pipe bubbling. Figure 9 below shows
the reaction stopped & the bubble dissipated.

Figure 9
The solution is now decanted (poured off) or filtered but pouring off is usually sufficient. What
is left is copper remaining at the bottom of the beaker. This is shown below in Figure 10 &
Figure 11.
Figure 10
Figure 11
 Next the solution can either be boiled outdoors in a round bottom flask until fine white
fumes appear, this can be difficult to spot. The clear solution is poured into a round bottom flask
& placed in the heating mantle, no other glass ware is used for this. Upon the proliferation of
white fumes, the heating mantle is turned off & the solution is allowed to cool. From here the
solution can be distilled in the same set up as outline in the drain opener distillation explained
above.
If distilling the dilute solution, a lot of water will be carried over to be removed prior to
collection of concentrated acid. This was not saved for future distillations.
Regardless of boiling first or going right to distillation, this process required the removal
of much more water before collecting concentrated acid. The distillation will have the same
stopping point as above & same testing on the paper as above. Figure 12 below shows the
clear/lightly tinted blue solution in the flask prior to boiling.
Figure 12

Both methods of reducing the water content REQUIRES the using of boiling stones, even
so, I would still sometimes get violent bumping to the point that sometimes it would jet hot acid
out the top of the flask. PPE MUST be worn, & rinse water must be on hand in the event there is
contact with the hot acid. This should be done over a surface that can contact acid, I used an old
school desk so that I did not potentially ruin anything of value to me.

When the Pt electrode was used the green dilute solution was made, I found this to be less
ideal than the clear solution as it did stain my glass ware, it took many rinsing’s with water or
dilute nitric, or dilute sulfuric acid to clean my round bottom flask. After this I made sure to
leave more solution in the flask when determining my stopping point for the remainder of the
dilute acid I had on h&. After this experience I switched to only using the lead electrode as I
found it far superior. Figure 13 below shows the white smoke stopping point for boiling & there
is splatter on the heating mantle as a result of bumping & hot acid erupting out of the mouth of
the flask.
Figure 13
Figures 14 & 15 below show the stains on the glass ware, this is fine for future experimentation,
but I prefer to maintain my equipment & would like to keep it clean & free of stains.
Figure 14
Figure 15
If possible, the lead electrode should be used over the Pt electrode.

HNO3 Distillation:
Equimolar amounts of H2SO4 & KNO3 are weighed out. If using Drain opener as the H2SO4
source, I recommend using drain opener over using clean H2SO4. For a 500 ml flask I typically
add one mole of each & 50 ml of water. Do not go above 147g (1.5 mol) of H2SO4 as to not
overfill the round bottom. Place the round bottom in the heating mantle. Using a funnel add in
the KNO3 then the water & next the H2SO4 is slowly & carefully added. The set-up of the
distillation apparatus is pictured below in Figure 16, it is very similar to figure 1 for the H2SO4
distillation except the plastic or metal keck clamps can be used for this distillation, a short piece
of tubing can be (& should be in the event distillation is not performed in a well-ventilated area)
added to the 105o elbows vacuum arm. This tube should be fed to a beaker of water where
(similar to the Birkland-Elyde reactor) the nitrogen dioxide (NO2) gas produced will bubble
through the water leaving dilute HNO3. Also needed is a bucket with cold water, the tubing &
the pump. The cold water is fed in through the bottom of the condenser (the end near the product
discharge) & returned to the bucket through the top. The idea being that the coolest water is at
the distillate discharge end.
Figure 17

Begin heating the mixture. When KNO3 & H2SO4 are mixed the produce HNO3 & KHSO4. As
the distillation progresses some of the KHSO4 will precipitate2 out of solution, this is fine &
normal. As the solution is heated, a red gas will form. This is nitrogen dioxide (NO2) & is not to
be inhaled. As the distillation progresses less NO2 will be produced & distillate will begin
carrying over at a faster rate. See figure 18 below for what the HNO3 distillation will common
look like mid distillation, the red NO2 gas has all but disappeared but the solution has a yellow
tint, this is okay. The finished HNO3 may have a slight yellow tint to it. The final product should
be stored in amber glass bottles.
Figure 18

There is no density change to look for in this distillation, instead the distillate must be
periodically tested for strength. The videos labeled Strong HNO3, HNO3 test, & Dilute HNO3
show how a piece of copper behaves differently in each solution. Like the H2SO4 distillation, it
is better to have a lower yield that is more concentrated than a higher, more dilute yield,
consistency/repeatably is the name of the game here. The heat is turned off when the level in the
flask appears as shown below in figure 4. This is what it will look like when the HNO3 has been
removed & only the precipitate remains. Towards the end of the distillation there may be a small
resurgence of the red NO2 gas as seen below in figure 19.
Figure 19
Figure 20 is another picture of the first nitric distillation. When the flask has been lifted there is
bubbles/foam on the top & some liquid remaining at the bottom. The H2SO4 distillation should
have about the same amount of liquid remaining in the bottom.
Figure 20
Figure 21 shows the cooled flask with the KHSO4 solid salt remaining.
Figure 21
 The Acid collected in the collection beaker is labeled “Dilute Nitric” & will be redistilled.
Several batches of this can be ran & collected. The KHSO4 left in the 500ml round bottom
boiling flask is allowed to cool & is then carefully removed by rinsing the flask with hot water,
careful not to shake the flask too hard & break it. Typically filling the flask with warm to hot
warm & swirling around will start to dissolve & break up the salt. Fill, swirl, dump, & repeat.
This salt is hazardous, & the solution of water & salt (or just the salt) should not be ingested nor
contact the skin or eyes.
After collection, a second distillation is performed. This time there is less NO2 gas
produced. If using a three-way connector & thermometer, collection of concentrated acid should
begin around 118C. If using a 70o elbow, you will need to test periodically. (The three-way will
also need to test, but only after reaching about 118C) Test the distillate periodically with copper
to see how strong it is. Collect until flask is nearing dry** & turn off heat.

*If using the Birkland-Elyd reactor method, expect to remove a lot more ‘dilute’ acid as the
concentration of the acid produced is much lower than if using H2SO4 & KNO3. This should be
disposed of & not saved for redistillation.
** during 2nd distillation, sometimes the remaining 10 or so ml remaining in the flask do not
appear to be boiling & no distillate is being collected. This is likely H2SO4 that was unreacted &
distilled over with the first batch. Distilling this over with your HNO3 will result in poor tests
with the HNO3 & copper as when HNO3 & H2SO4 are mixed the resulting nitrating mixture
does not react well with copper. I usually will redistill this with the next batch of HNO3
watching & test carefully. This is likely due to improper measurement when measuring the
KNO3 & H2SO4, it is better to add too much KNO3 than too much H2SO4.
2: Precipitate, meaning the salt produced (K+ SO4- are positively & negatively charged combining to form a salt) will fall out of solution
appearing as a white clump in the bottom of the round bottom.)

Storage of acids: Both acids should be stored in amber glass bottles.

Nitration of Cellulose:
Nitrocellulose (NC) is the technical term for smokeless powder. Cellulose is often found
as paper products (Towels, napkins, printer paper, etc) or 100% cotton products, as well as many
other products. The ideal version of cellulose for this project is microcrystalline cellulose
(MCC). Which is sold as a supplement online, but paper towels & printer paper have also
worked in the past. I will focus on MCC & 100% cotton, not on paper towels for the time. When
cellulose is added to a nitrating solution it becomes nitrated giving it the properties that make
gun powder so special. The nitration solution is an equimolar composition of HNO3 & H2SO4
that have been chilled. One mole of H2SO4 is added to a 250 ml beaker & one mole of HNO3 is
stirred in slowly with a stir bar on a magnetic stir plate or (though less ideal) with a non-reactive
(Stainless steel or glass) stir rod. The slow addition is so that the solution does not get too warm
& run away3. The beaker must be placed in an ice bath to prevent a run-away. In the event of a
run-away reaction, the solution with rapidly boil & erupt hot acid & NO2 fumes. I have had this
happen when making nitroglycerin more than once. The solution was quickly quenched with
cold water, the reaction/glass ware were cleaned up & the process started all over.
3: A runaway reaction is A thermally unstable reaction system which exhibits an uncontrolled accelerating rate of reaction leading to rapid
increases in temperature & pressure. Basically, it gets too hot a decomposes. In my experience you lose the batch, it gets hot & then boils over, &
you see a red nitrogen dioxide cloud form. Dilute with water & pitch. Start again ensuring the reaction is performed cool in an ice bath.
Microcrystalline Cellulose Method

For each mole of acid used weigh out 18 grams of MC cellulose. The MCC is carefully &
slowly added ensuring there are no clumps formed & it will sit in solution for 18-24 hours. See
the video labeled “MCC Nitration” for instructions on the addition. The MCC should be weighed
out & added over a screen or with a flour sifter added very slowly as shown in the video to avoid
clumps. Ideally this is done on a stir plate in a beaker with a stir bar to effectively add the MCC
without clumps. Less ideal but better than hand stirring is placing a beaker in the heating mantle
& stirring using the stir function of the heating mantle as depicted in the video. If stirring by
hand, the cellulose should be added in very small quantities & thoroughly stirred. As more MCC
is added, the solution will thicken up & stirring with a stir bar may become difficult.
The procedure for operating a stir plate is as follows, place the beaker in the heating
mantle add the medium sized stir bar, too small & as soon as the solution thickens the stirring
will fail, too large in the beaker the stir bar will be too far from the magnet & fail as the solution
thickens. This is why a stir plate (flat surface) is preferred using a beaker).
Both acids are chilled in an ice bath, this can be a deep pan or dish, I use a 9 inch by 9-
inch baking dish. Cold water & ice are added to the dish such that the beakers with small
quantities of acid will not float or tip over but enough that the acids will be chilled down. Tare
the beakers on the scale & weigh out one mol of sulfuric acid (H2SO4) which is 98 g of sulfuric
acid into one beaker & one mole of nitric acid (HNO3) which is 63 g into another beaker. One of
the beakers should be large enough to hold both acids without filling one of the beakers more
than half full. I do not recommend large batches but if this process is to be scaled up the excel
spread sheet is contained in the file package to assist.
The two acids are chilled in the ice bath. The smaller of the two beakers is poured into
the larger beaker slowly after resting in the ice bath for several minutes. When mixing the two,
the acid should be added very slowly & stirred in as to not heat the mixture too much. Upon the
acids being mixed they are left to chill for several more minutes in the in the ice bath. The
mixture is then placed in the heating mantle or stir plate & a stir bar is added. The MCC is
weighed out, again 18g of MCC per mol of acid (one mole H2SO4, one mol HNO3, 18 g or 2, 2,
36g). More MCC CAN be added but I found it difficult to stir. The stir function is clicked on &
the stir bar can be observed slowly stirring. The speed is slowly sped up to a moderate speed.
Too slow there may be clumping too fast & the stir bar may come off course. If the stir bar
comes off course, it will be observed bouncing around in the mixture opposed to spinning in a
circle. In the event of this it is turned off, recentered in the beaker, clicked on & slowly speed up,
possibly to a slower speed. Holding a flour sifter or screen over the beaker, the MCC is
scooped/poured on to/ into the screen/flour sifter in small quantities. The screen is lightly tapped
on the edge, or the flour sifter is operated. This should be performed outdoors. See the video in
the videos folder detailing this. If a stir bar is not available & hand stirring is to be performed
less MCC should be added & sprinkled in as if taking a pinch of salt & salting food
(rubbing the thumb & index finger together) & more thoroughly stirred to avoid clumping. Once
all the MCC has been added to the mixture it is stirred for a few more minutes & the mixture is
removed from the stir plate & allowed to rest for 18-24 hours. Figure 22 below shows the MCC
slurry in the acid.
Figure 22
Post Nitration Processing

After 18-24 hours the mixture is poured into a large beaker (1000 ml filled about
halfway) with cold water & the beaker rinsed to remove any nitrocellulose stuck to the walls in
the beaker. The mixture is stirred & the water decanted or filtered off. The now nitrated MCC is
MCNC or multi crystalline nitrocellulose. The MCNC is rinse several times with cold water &
then 2-3 times with a 2% sodium bicarbonate (baking soda) solution. 20 grams of sodium
bicarbonate are added to 1 liter of water. Upon rinsing 2-3 with the sodium bicarbonate solution
the MCNC is added to a pot & more of the 2% sodium bicarbonate solutions is added. This
mixture is boiled (a low simmer) for 15-20 minutes. The mixture is allowed to cool & the MCNC
is filtered off & left to dry. Drying can be sped up by placing the MCNC in the oven at about
93C for 15-20 min or until dry & powdery/crumbly. Figure 23 below shows the MCNC in the
sodium bicarbonate solution prior to boiling.
Figure 23

Figure 24 below shows the wet MCNC being poured through the filter.
 Figure 24

Figure 25 below shows the MCNC after filtering set out to dry.
 Figure 25

Figure 26 below shows the MCNC after drying.

Figure 26
Testing
A small pinch of dry NC is ignited & can be compared to video labeled fast MCNC & CFE
Pistol which is a commercially available powder for loading 9mm ammunition.

Making a double base powder (A faster powder)

Double base powders burn much faster than single base & are often used as pistol cartridge
powders. They require the use of nitroglycerin.

Making Nitroglycerin
Glycerin is nitrated in a similar manner as cellulose with a 1:1 mole ratio of HNO3 added to
H2SO4. Both acids are chilled prior to addition & placed in an ice bath while mixing. While
adding the HNO3, the H2SO4 is stirred. Ensuring the solution remain cool, the glycerin is added
slowly, for a 1 mol batch 30g of glycerin are added. Note: more can be added but is not
recommended & has not been tested, this will be a waste of some acid but for safety reasons.

***It is highly recommended to make the nitroglycerin (NG) in small batches as this is a very
powerful substance*** If larger batches are made, they should be split up into several containers.
NG is stored underwater in a cool dark place & try & use it quickly. It will be fine in storage, but
I don’t like to, NG is very powerful. I make it & try & use it ASAP.

Please see my videos regarding NG & show the utmost respect for it as it can be very dangerous.

Procedure:
Like the cellulose nitration, one the acids are placed in a large enough beaker to hold both
the acid plus the glycerin. The two acids & the glycerin are weighed out & placed in the ice bath.
After chilling for several minutes, the acids are slowly mixed while stirring as to not heat them
up too much. They are allowed to chill for several more minutes & the glycerin is slowly added
while stirring. The batch outlined below is rather large & smaller batches should be made for
safety. Rather than 30g HNO3, 50g H2SO4, & 15g glycerin, a safer batch would be along the
lines of 15g HNO3, 25g H2SO4, & 7g.

30 g of HNO3 are weighed out as shown in figure 27 below.

 Figure 27

50 g of H2SO4 are weighed out as shown below in Figure 28.

Figure 28
15 g of glycerin are weighed out as shown below in Figure 29 below.
Figure 29
The two acids & the glycerin are placed in an ice bath & allowed to chill for several minutes.
The acids are slowly mixed as to not heat the mixtures too much & then the mix is allowed to
chill in the ice bath for several minutes & this is to be performed outdoors. The glycerin is
slowly stirred in with a glass of stainless-steel stirring rod. This is not added to quickly as the
reaction may run away. Once all the glycerin has been added the mixture is allowed to react for
30 minutes. It will have an oily appearance on the surface of the acid mixture as shown below in
Figure 30.
Figure 30
 Upon completion of the reaction, the acid/NG solution is poured into a beaker of cold
water. Typically, I would fill the 1000 ml beaker half full of cold water & add ice before mixing
in the glycerin so that I had cold water on hand in the event of a runaway reaction. It was not
filled with ice, just enough to chill the water & the ice would all be melted by the time the
reaction was complete or was removed by hand after the reaction was complete.

NOTE: in the event of a runaway reaction DO NOT try & pick up the beaker & pour into the
water, pour the water into the beaker, filling it & allowing it to overflow into the ice bath.

After the reaction was complete, it is poured into the beaker of ice water. Small droplets
may be floating in solution, stir the mixture to knock these to the bottom by stirring. After
stirring you may see an oily substance on the surface, this is will not fall out & that is okay. The
reaction beaker would be rinsed with cold water & poured into the beaker. The larger ice water
beaker is stirred again, the NG will be a visible white blob at the bottom of the beaker. If it is
clear or not present something went wrong & try again. Figure 31 below shows the NG at the
bottom of the beaker, this is what I considered a “Large” batch, what was made from the pictures
above using 30g HNO3, 50g H2SO4, & 15g glycerin.
Figure 31
 The cold water is poured off the top of the NG leaving enough water to cover the NG, it
is rinsed with cool water 4-5 more time & then with a 2% sodium bicarbonate solution to
neutralize any remaining acid. The NG is stored under water in a cool dark placed & to be used
as soon as possible. If exposed to light, over time may become unstable & turn to a yellowish
color. This is not something I would keep on hand. It can be stored for in the cool dark place for
a while, but I would make it & use it later that day.

Polymerization of Nitrocellulose

The nitrocellulose in then polymerized in acetone. The mixture of NC to NG is a 60:40 ratio

meaning for every 60g of NC added to the acetone, 40g of NG is added. This is what I found to
yield a fast enough burn rate to function when loaded into a 9mm case with a 125 grain (gr)
bullet in the FGC-9 without running out of case capacity nor resulting in an over pressurized
round. Like various methods of making acid & NC, various ratios & loading will be explored in
the future.
For this batches could be as large as I wanted as once the NG was added to the NC &
acetone it was rendered safe. I had conducted various tests with the NG before & after being
added to the NC & acetone solution. Prior to being added it could be set off by friction or impact
such as being hit with a hammer. There is a video in the videos folder showing a drop or two of
NG on a piece of paper & being struck by a hammer. After the addition to NC in acetone &
drying it could not be set off by the impact of a hammer nor friction, only heat/open flame. The
NG is measured by the number of drops from a pipet that I had. I would fill another beaker with
water, suck up the NG in the pipette & count the drops of NG that were transferred to the other
beaker of a water. Since NG is a white liquid, I would suck it up & begin dropping it out, if there
was water in the pipette, it should float to the top & I would only count the drops that left a small
white blob in the bottom of the other beaker. This gave me a rough count of the drops I had at
my disposal. One drop is equal to 0.05ml1. for every gram of NC about 75ml of acetone is used.
If the mixture appears thick more acetone can be added to thin it out & help dissolve more the
NC but not all the NC will dissolve, there will be some left in the beaker undissolved. The
calculation of NC to NG is as follows if starting with NG; 5 drops of NG multiplied by 0.05ml
per drop multiplied by the density of NG which is 1.6g/ml. drops cancel with drops & ml cancel
with ml leaving the result with the unit in grams. In this case 0.40 grams. For a 60:40 ratio, 0.60g
NC is to be used. If starting with NC the calculations are as follows; 1.450g NC divided by 0.60
equals 2.42 total grams. 2.42 minus 1.450 equals 0.967grams of NG to be added. 0.967 grams
divided by 1.6 g/ml, then divided by 0.05ml/drop. Grams cancels with grams, ml cancels with ml
& drops are left as the unit. In this case it equals 12.1 drops, in this instance I rounded down to
12 drops. If I had 12.5 I would round up to 13 drops. The excel spread sheet aids in this
calculation, I prefer to start with drops oppose to rounding down or up.
1 This is based on the density of NG & the approximate volume of one drop of water. NG has a density of is 1.6g/cm^3 or 1.6g/ml. The a
approximate volume of one drop of water is 0.05ml. The NG is added to the NC up to 40%. We are using XX% for loading 9mm. 1g NC there
for gets 0.XXg NG. Number of drops = (1drop/0.05ml)*1.6g/ml*0.XXg. grams & ml cancel out & you’re left with XX drops. Refer to the excel
spreadsheet for calculations.

Figure 32 below shows an example of my calculations.

 Figure 32

The acetone is poured into a beaker & the beaker is placed on the stir plate or in the
heating mantle & a medium sized stir bar is added. The stir function is turned on to a low to
medium speed & the oven or toaster oven is preheated to about 93C. After calculating the
amount of NC & NG to add, the NC is slowly stirred into the acetone & allowed to dissolve into
solution.
Figure 33 below shows the acetone in the beaker being stirred with the stir bar while the NC is
added.
Figure 33

Figure 34 below shows the acetone & NC solution being stirred.

 Figure 34

Most of the NC will dissolve but not all of it will. The solution is thoroughly stirred for
several minutes & checked to see how much NC is left undissolved. 10-25 ml of acetone can be
added to see if there was not enough acetone added but, unless the solution is very viscous it
should be fine. Figure 35 below shows about how much NC will be left undissolved.
Figure 35

The solution is stirred once more for several minutes & if no more NC is dissolved the
NG is pipetted in counting the requisite number of drops from the calculation. If more than
calculated is accidently added, the calculation is redone & more NC is weighed, added, &
thoroughly stirred in.
After the addition of NG a small flat surface with a small lip such as a coffee can lid is
lined with parchment paper, this is not necessary but makes removal of the plastic sheet much
easier. The ideal set up has the parchment paper lying flat across the surface of the pan/coffee
can lid. The lid is placed in the oven & the acetone solution is poured on to the parchment paper
until the liquid is about 3mm deep. It is allowed to evaporate in the oven until completely dry.
The lid is removed from the oven & allowed to cool. The plastic sheet is then peeled off the
parchment paper or scraped off the pan or lid with a scraper. This is done until all the liquid is
poured out of the beaker & only the undissolved NC & stir bar remain at the bottom of the
beaker. Figure 36 below shows the lids in the oven drying. It should be a thin yellow-ish plastic
like sheet. If it dries & appears as if it looks like a white powder, the solution may be thin & a
thicker pour is poured on the parchment paper. The white powder can be scraped off &
redissolved into the acetone.
Figure 36
 As shown above, the parchment paper is not laying entirely flat which is not idea but will
work.
Figure 37 below shows the plastic sheets after drying & coming out of the oven.
Figure 37
Figure 38 below shows the plastic sheet removed from the parchment paper.
Figure 38
 The plastic sheet is cut or torn into small enough pieces such that it will fit into a pill
bottle or similar type container & stored for further processing.
The last step is to use a pair of scissors to cut the plastic sheet into a fine powder. With
the 60:40 ratio I found with a good, sharp pair of scissors I could not cut the powder too small.
One hand held the pill bottle while the other hand operated the scissors. The pill bottle was held
at about a 30-degree angle & rotated in a circle while the scissors were operated. Cutting is
finished when the powder is small enough that a powder charge will fit into a 9mm case. I was
never able to cut it too small with this method, only not small enough. If the powder was not cut
enough the requisite powder charge would not fit into a 9mm case.
Figure 39 below shows what the final powder should look like when cut small enough, again, a
safe load should fit in the case without filling it to the top.
Figure 39
Loading:
Please refer to “But what about ammo Vol 2” for more guidance on loading procedures.
In general, handloading should be done free of distraction, carefully, & everything should be
well documented.
If you choose to follow this guide know that you are the only person responsible for your
safety. Each individual should work up their own load. The following information is a starting
point. I would not go less than the outlined charge nor more than it. I will note that I have had
over pressurized cases cramming a lot of powder into a case, never to the point of disaster but I
have had some bulged primers. I have found through testing that there is consistency between
batches meaning that following the same process to make the NC, NG & mixing the two in the
same ratios (even with different quantities, i.e. one batch was made with 1.450 g NC & 12 drops
of NG, a 60:40 ratio & another batch was made with 8 drops of NG & 0.96g NC, again, a 60:40
ratio). The first few batches I made were all remote fired for safety. After that the first round
from each batch was remote fired. While this is still in development/beta recommend users
remote fire until they feel comfortable & even then, be mindful how close their hand is to the
chamber. I have not had any catastrophic failures with this method, but safety is the number one
priority.
Using range pick-up once or twice fired brass a variety of small pistol primers & 125gr
bullets I found that the minimum loading to cycle my FGC-9 was 4.1 grains & I began to see
signs of over pressure (bulged primers) at 5.2 grains. I found that a load of 4.2-4.8 was ideal &
5.0 at the max. If users choose to use a different bullet weight, please document your load data &
cautiously work up the load. Figure 40 below is the bulged primer from the loading of 5.2
grains.
Figure 40
FAQ:
Q: Why make smokeless powder in the first place? Why not use black powder?
A: Although black powder is easier to make & less involved, smokeless powders is required to
properly operate semiauto firearms. Black powder will quickly foul the action of a semiauto
firearm & produces a cloud of smoke.

Citations & acknowledgements

I would like to thank the following people for their help in no particular order.

CathodeG
Austin Jones (Sword of Gidion)
Opitimus.Synthesis
InCarbonite/Mendez3DArmoryBot
AGLeaks/FedPlots