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Making Sodium Chlorate Black Powder (2nd Edition)

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It is simple, easy to obtain materials and fairly powerful. A homemade Chlorate Black Powder making manual that comes with decent makeshift fuse making and discussion on Chlorate-Sulfur known issue. For a desperate situations when it is needed. *This documentation is the improved version of Making Sodium Chlorate Gunpowder.
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Making Sodium Chlorate Black Powder (2nd Edition)
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  • Making Sodium Chlorate Black Powder

    (2nd Edition)

  • 1

    Making Sodium Chlorate Black

    Powder (2nd Edition)

    By: arefiq

  • 2

    Table of Contents:

    # Subject

    Page

    1 Preface

    3

    2 Abstract

    4

    3 Introduction

    5

    4 How does Black Powder works

    6

    5 Materials and method implemented for the Chlorate Black Powder production

    7

    6 Be focus and Safety first. Again, use your common sense

    8

    7 The Chlorate Black Powder in 1788 brief history

    9

    8 The Chlorate-Sulfur mix notorious issue

    10

    9 Chlorate-Sulfur study by Herbert G. Tanner

    11

    10 The main highlighted information from the study

    15

    11 The Polythionic acid Trigger mechanism

    16

    12 Discussion of the Trigger mechanism

    17

    13 Getting started, getting the right materials and explanations

    19

    14 Homemade Chlorate Black Powder process

    23

    15 The makeshift kitchen tissue strip fuse

    25

    16 Chlorate-Sulfur mix and Chlorate Black Powder decent sensitivity test

    27

    17 The typical burn rate test

    32

    19 Reference and recommended reading

    37

  • 3

    Making Sodium Chlorate Black Powder (2nd edition)

    By: arefiq

    It is simple, easy to obtain materials and fairly powerful. A homemade Chlorate Black Powder making

    manual that comes with decent makeshift fuse making and discussion on Chlorate-Sulfur known issue.

    For a desperate situations when it is needed. *This documentation is the improved version of Making

    Sodium Chlorate Gunpowder.

    Preface: In the name of Allah, Most Gracious, Most Merciful; peace be upon you,

    Since I was a child Im always fascinated by those simple exploding tubes device called firecracker. Since

    it is actually a banned item it is hard to find them other than the festive days. Even most of them that

    sell on market were actually smuggled, and expensive enough to afford. Then, my search starts on

    making one myself. There goes Mr. Google. Of course making, handling, storing these is dangerous since

    it is explosive and can cause potential fires. Use common sense, general knowledge with the chemicals

    hazards and also safety first.

    There is also other guide on making real Black Powder here on the net; however since here where I live I

    could not get myself on certain materials and the chemicals I need especially the oxidizer Potassium

    nitrate. Therefore, I am here writing the guide based on my experience how I make one here where I

    live by using Sodium chlorate as oxidizer substitute.

    One will think that this person will blow himself up and ended with broken or lose his limbs because

    mad enough to substitute Nitrates for Chlorates in making Black Powder. Yes, I am mad enough to

    experiment with it. Thanks to Allah that I am still intact with no broken or lose limbs after all those

    years. I aware the danger it poses, the compatibility issues, and the sensitivity issues of mixing Chlorates

    with Sulfur is a recipe for disaster. However I did succeed on making one that I consider it is for

    desperate situations. Every method employed here is not safe and dangerous because working with

    Chlorate-Sulfur mix. Of course, use common sense and safety first.

    Frankly odd enough, the way the Chlorate Black Powder made never just yet to set off by itself while in

    storage as long as I remember even the longest one on the shelf about more than a couple of years. But

    that did not cancel the possible self-ignition issue of Chlorate-Sulfur mix potential as we all believe. We

    think it is safe, until something went wrong. It seems its just not there yet. However, here the Chlorate-

    Sulfur issue will be discussed further in details.

    I am aware that I am not a professional in this field of study to write a guide and my experience in

    handling and utilizing such explosive powder. And I always consider myself as an amateur and still need

    more to learn. Most of the knowledge I gain is from reading materials and some from personal

    experiences. Again, I am not an expert in this field. I am not a Guru, Sensei, Sifu, Teacher and or a

    Scientist that utilizing proper tools and instrumentations or also not limited to any of those terms ones

    use to describe these kinds of people. I dont belong to any group of pyrotechnic nor receive any

    pyrotechnic training and or having any qualification regarding the field of study. I am just a typical

    country guy lives far from big cities which work individually that fascinated by the arts of Black Powder.

    arefiq

  • 4

    Abstract

    This homemade version of Chlorate Black Powder is simple, easy to make with available materials, and

    explode with fairly loudness and strength. However, flash powder made from Potassium perchlorate

    and Aluminum powder provide much more power, safer handling, and much faster burning rates and

    produce louder report than the typical Black Powder. Despite that, we proceed for producing Chlorate

    Black Powder due to the unavailability of materials and or when in the times of desperation whenever a

    Black Powder substitute is needed to be utilized on the field. Generally Chlorate Black Powder would

    produce much more power capacity than a Nitrate based Black Powder.

    This is not the full, the best and complete guide on homemade Black Powder but it still works. However,

    bear in minds that safety come first, use common sense and acquire the knowledge and information of

    making Black Powder before made the powder practically. This document covers the subjects of

    producing Sodium Chlorate Black Powder, the Chlorate-Sulfur known issues and producing makeshift

    fuse.

    This version of documentation is the continuation from the results of experimenting and optimizing

    from my older documentation of Making Sodium Chlorate Gunpowder which need improvements. This

    guide is not limited to Chlorate only oxidizer base. Also good enough for Potassium or Sodium nitrates

    based and should be complying with its chemical safe handling and precaution. I would not be

    responsible in any liability of your doing regarding this documentation. Read it at your own risk. Making

    a Black Powder is a dangerous business. This documentation is for reading, educational, information,

    optimization, learning and sharing purposes.

    *I thought at first it would not be necessary to update my former documentation posted on 2009 (when I was still

    a kid), however; with over than 8000 views (thanks for take a look), it really concerns me. Therefore, here the

    further improved method and a little more information is included (at least, this time much better than before).

    This documentation is just a small fraction from the intentional documentation, hope more will be coming in the

    future. Allahs willing.

  • 5

    Introduction:

    By means of desperation, one would result from failing to obtain the preferable oxidizer of Potassium or

    Sodium nitrates. Thus, substitute the oxidizer role with other type of oxidizer which is readily available.

    Or the desperation calls when in the state of war or state of emergency where to obtain materials

    needed is limited and manual old time production of Nitrates would take longer time. In addition to

    that, high explosive is out of reach to be utilized and high explosive require detonator to work

    effectively. The desperation calls comes with a price, which is obviously to work with the dangerous

    Chlorate-Sulfur mix of powder.

    Today in modern times, people assume Low-Order Explosive is weak and out of question to be used for

    material damage and fatal injury. In fact, back in the history the common Low-Order Explosive device

    Pipe Bomb was notoriously utilized against personal and materials in an unconventional warfare. It has

    been favorites of revolutionaries and criminals throughout the world. Other than that, Black Powder still

    capable to produce considerable blast energy many kind of rocks in rock blasting. Is fireworks is not

    capable enough to kill people and cause damage? Just imagine if those huge aerial fireworks shell that

    we used to watch during festive days explodes in ones house. Therefore, a properly made Low-Order

    Explosive device still poses a serious threat even it might not be as powerful as High-Order Explosives

    counterpart.

    In older times, the secret of making Black Powder lies in the charcoal used without excessive

    temperature in making. Also, the method to mix the powder is vital. People said that, the best wood to

    make a charcoal for Black Powder is from the softwood types of Willow tree species. Other types of

    softwood also can be used to make a good charcoal for Black Powder as such Pine wood and even from

    the grape vines.

    However, the method to produce the Black Powder is varied. Some said it has to be ball milled no other

    way to produce high performance homemade Black Powder. Other implements the well-known CIA

    method. While other employs the Precipitation method and some commercially made powder uses Hot

    Aqueous Saturated Mix method and Wet method. Nevertheless, here in this documentation the Wet

    method is preferred because to avoid dry mix impact and heat in the procedure that might cause

    tragedy in making the very sensitive Chlorate Black Powder. Although the method used here has slight

    changes were modified to the method to comply with the very sensitive mix and also for the ability of

    homemade production with available apparatus.

    If ones want to produce a high quality, high performance and the fastest as possible homemade Black

    Powder with Nitrates, there is a lots out there on the net on how to making one. From simple to

    advanced and even a much more expensive approach. Yet, none of Chlorate Black Powder was made. I

    believe there is somewhere out there. Nevertheless, in old times they still capable to make a quality

    powder where advanced scientific machines were unavailable with decent unknown purity of materials

    and decent accuracy. Some Black Powder enthusiast might be exaggerating with their method and

    materials selection of choice for the best while other might be bias and some other might never even

    make one or even test with it thus concluding and post all their claims based on just an info from a mere

    reading. I recommend reading on Black Powder Manufacturing, Testing & Optimizing by Ian Von Maltitz.

    This book clear various misunderstood regarding the Black Powder and how to produce a good, high

  • 6

    quality and performance with the fastest burn rate powder possible and some even surpass the

    commercial made powder. However, the book did not state on how to make it specifically with

    complete procedures but it included the critical factor that affect the Black Powder performance. Other

    than that, it includes results of data from various tests, many other interesting subject and very

    informative for further insight.

    Initially, Black Powder was used for propelling a projectile. In history there were once that Black Powder

    was used for blasting rocks. However it is not so powerful and brisance enough for specific more

    intensive purposes and later was replaced by better and stronger explosive, a dynamite. But still, one

    can benefit its power properties to be utilized when needed utmost. Plus, it is way cheaper than high

    explosives.

    In my older document Making Sodium Chlorate Gunpowder, I state it as gunpowder. However, I change

    it to Black Powder because the term gunpowder sounds to be closely related for a powder to be used in

    gun which is not the case. Either way, there is no distinct difference between the two terms as it is the

    just the same.

    How does Black Powder works

    A gunpowder or Black Powder is an intimately mixture of oxidizer, fuel and sensitizer. The common

    recipe which is still acceptable composition around for general purposes is 75:15:10 formulas by weight

    of Potassium nitrate, charcoal and Sulfur. Since here we utilizing Sodium chlorate for the oxidizer role,

    generally the powder would produce a faster, stronger, violent and way much more sensitive than Black

    Powder made with the original Potassium or Sodium nitrates. Faster and stronger doesnt make it a

    safer and perform better in certain task, also comes with significant payback which is highly dangerous.

    Black Powder is considered as Low-Order Explosive. Because it cannot explode by itself in an open

    space, instead it burn or deflagrate at high rates. When in closed and confined state, the powder burns

    inside very rapidly and build up gas pressure strong and fast enough thus resulting the tube body to

    rupture and explode. The faster the burning rates of the powder, and the stronger the body container to

    hold the gas buildup until all the powder were burnt inside, the stronger the gas explosion to occur.

    However, it will only explode when the powder has sufficient or excess amount of powder to convert to

    gas and the pressure is strong enough to cause the casing to rupture and thus exploded. As in simple

    terms; a gas pressure blast. For the explosion to works properly; the faster the powder burn rate, the

    better it serve its purpose.

    If the powder is not sufficient to build strong enough pressure and the container hold strong enough to

    resist, the container will not explode, but rather the gas will leak at the weak spot as the gas pressure

    escapes at high speed. This is preferable for propelling a projectile like in the Muskets rifles barrel.

    By chemical reaction or equation, one cannot guess the true or the exact product of combustion of Black

    Powder. Because the exact chemical formula of the charcoal used is unknown. A charcoal is not a pure

    carbon. In the art of making of high performance Black Powder, specific charcoal from specific types of

    wood used to make charcoal is vital to produce the highest burn rates possible. The charring process

    also counts to retain the other substances that reside inside which called volatiles. These volatiles is

    actually vital in the reaction with the incorporated materials notably the oxidizer and the Sulfur as it is

    believed.

  • 7

    Generally Chlorate based Black Powder is not suitable for shooting in musket because it tends to

    corrode the barrel. However, if desperation calls its still works to propel the projectiles as it should be.

    This powder is effective in low-order explosive device. Remember, it is a low-order type of explosive. It

    depends on gas pressure buildup in confined condition to explode. It did not detonate to cause massive

    high explosion as high explosive would. Good thing is that, it does not require blasting cap or detonator

    to start the explosion however; it is highly heat, sparks, friction and impact sensitive. Plus if the powder

    is getting wet, the performance and its sensitivity would decrease.

    Materials and method implemented for the Chlorate Black Powder production

    Here in this documentation the main materials used for the Chlorate Black Powder is as follow to comply

    with materials availability in the area of neighborhood:

    As the desperation calls this is not considered to be the best result of Black Powder as its not utilizing

    the best or a good choice of charcoal for the purpose.

    In my experience, I mostly made 100g of powder batch at a time due to my tools limitation. Also, it is

    generally better to work in small amount.

    75% by weight: Sodium Chlorate (99.0% purity), powdered +sieved

    15% by weight: BBQ Charcoal briquettes, powdered +sieved *I suspect might be made from

    coconut shell as the package did not include what the charcoal come from, plus coconut shell

    charcoal used extensively as source of charcoal. No any other additives such as petroleum based

    product or quickening agent to start fire as it states.

    10% by weight: Sulfur flour, already in powdered form +sieved

    Note: Yes, I aware that utilizing a BBQ charcoal briquettes is the worst possible choice for a charcoal.

    Plus if it is true the charcoal come from the coconut shell which is considered as hardwood it is way

    much worst choice charcoal for even a fairly Black Powder.

    However, I say it is still in usable range despite its poor performance. It burns in violent flash rather than

    just a slow burning. It is so sensitive that even a small unseen ember could ignite it. In one test which

    will be discussed in detail in later section, results show that it burns at the rate 0.53 second in 20cm3

    powder train of 20cm x 1cm x1cm. Therefore, I calculate that it would go for 37.7cm per seconds. Its

    quite fast, but still poor in performance. As the burning resides, leaves with very few black residue, with

    airborne embers around. Thats not all; the key is that it is still can be improved further.

    Of course the flash speed is not even equivalent or near to a Flash powder mix as I suppose. Therefore, I

    pre-assume that if the Chlorate Black Powder were made with the prized softwood charcoal as such the

    Willow wood charcoal charred nicely for the job and proper milling of the charcoal, it would be amazing.

    I found on the net on how fast a Nitrate based Black Powder burn rate could go. The fastest I found was

    a Nitrate based Black Powder made from Black-Willow branch at amazingly speeds of 189cm per

    second! (Taken from: http://www.brianredmond.net/dwilliams/bptester/bptester.html) 5 times faster

    than a makeshift Chlorate Black powder! Wow! Crazy speed for a Black Powder! Maybe someone out

    there might capable to make even faster Black Powder burn rates.

  • 8

    The original recipe method was not made by me; instead I am just following the step and comply with

    my needs into producing the Chlorate Black Powder. Original method was taken from the net at Ulrich

    Bretschers Home Page > Ulrich Bretschers Black Powder Page, Homemade Black Powder. Yes, I amazed

    that those simple steps making homemade gunpowder actually works nicely for its purposes (Thanks a

    lot for sharing).

    Be focus and Safety first. Again, use your common sense.

    Safety comes first. But to tell the truth, you will get injured somehow because you are playing with fires.

    Burns would be common. I got several burn marks myself. So, be focus on whatever you are doing.

    As for me, I once got my hand serious burns and leave permanent burn marks because of the sparkling

    powder spew molten slag on my hands while experimenting and testing burn rates with different

    percentage of composition for Chlorate Black Powder. Although the burns healed, still leaves marks.

    Generally, some mild burns did not leave scar and would healed.

    Another serious burn when I accidently hold a very hot steel tube without knowing until steams of water

    actually came off from my hand! It was so careless that I didnt realize it. The cause, when I was trying to

    make my first rocket without the balancing stick, I put it in a steel tube and lit it hoping it will launch

    inside. But it fails to fly out. Instead, its just jets inside and actually heat the steel tube so hot and I hold

    it without realize it right on the spot where the jets stream is located! My palm sizzled with steam came

    off and instantly wrinkled my palm like a dried dead persons hand. The pain was very intense! I had to

    put my hands in cold icy water for the whole day to lessen the pain. The good thing, it didnt leave any

    scar.

    And the other day, when experimenting on making the fuse, I actually tried to dry them in an oven with

    just a warm normal temperature. At first it was fine; I thought it will be fine as long as the temperature

    not rise high enough. But I was wrong. After a while, it ignites! Inside the oven! In mere seconds the

    oven actually pop and explode to release the expanding gas pressure buildup inside. The whole house

    filled with thick white smoke. Thank to Allah, no one was home other than me. However, the oven was

    all covered in black inside out. I have to clean every inch of the oven parts. Chlorates are potentially

    poisonous. I dont want the next day my family use the oven to cook something then someone ate them

    and died because of chlorate poisoning! Well actually my mother did use it in the next day. Thank Allah

    again that no one get sick after eat the cooks! In which including me.

    Well, experience. We learn our lessons and gain additional knowledge. But make sure youre not crazy

    and mad enough to lose your precious organs or even ones lives.

  • 9

    The Chlorate Black Powder in 1788 brief history;

    Maybe the mill explosion was caused by sabotage? Well who know? If Berthollet successfully

    manufacture the more powerful Chlorate Black Powder, it will replace the Nitrate Black Powder from

    the market. This will cause huge liability towards the Nitrate Black Powder manufacturer.

    Nevertheless, information is not clear regarding the cause of how the incidence happens. In Davis book,

    The Chemistry of Powder and Explosives; it states that the mill was left alone; as the party (invited

    people to witness including engineer) went for breakfast once the mill was started. Two of the

    unfortunate that first to return; the material exploded. This concludes that the cause was because of the

    powder mix instability; notably by friction, impact and heat.

    And this enhances the explosion probability by the types of mill he used which is the stamp mill. Ian Von

    Maltitz states in his book shown that stamp mill was proven in history that it has a very bad reputation

    in Black Powder manufacturing. Many Black Powder manufacturing stamp mill known to cause

    explosion due to the violent stamping action of the mill itself, rather than a circular grinding motion

    action as compared to a mortar and pestle should. Powder milled in this manner always carried out wet

    to reduce ignition probability. Even so, numerous numbers of accidents still happen thus had been

    banned and phase out of services.

  • 10

    The Chlorate-Sulfur mix notorious issue

    Here some examples of common quotation that people use regarding the Chlorate-Sulfur mix:

    Never mix Chlorate with Sulfur! Its a Death mix! Recipe of disaster! Spontaneous ignition! Sudden

    explode! Highly sensitive! Unstable! While some other extremist employ a very offensive statement in

    which it is not necessary to be included here.

    And here is some of the reasoning and a possible cause why it is deadly mentioned by most:

    1. Sulfur and or Sulfides can react with Chlorates and form Chloric acid which is unstable explosive

    2. Acidic compound presence in Sulfur decompose Chlorate thus causing ignition

    3. Fine powdered Sulfur reacts with open air Oxygen to form Oxides of Sulfur which then reacts

    with Chlorates in the presence of moisture to form Chloric acids. Thus promote ignition.

    4. The presence of Oxides of Sulfur reacts with Chlorates in the presence of moisture to form

    Chloric acids thus promoting ignition.

    Yes, it is true at a point and the possibilities are there. However, on my opinion these were actually had

    been exaggerated more like a war propaganda to avoid people to utilize such a compound. Rather, it is

    actually was a misunderstood and the actual info transfer had changed from person to person in

    understanding how EXACTLY it works.

    In facts, this co called Death mix is actually had been used extensively. Notably in strike matches, in

    some Flash powder mix and not least to a commercial fireworks made by the Chinese.

    Here, the link for result of series sensitivity test of the Chinese Flash powder mix that utilizes Chlorate-

    Sulfur; A Safety Study of Chlorate Firecracker

    http://www.google.com.my/url?sa=t&rct=j&q=&esrc=s&source=web&cd=2&cad=rja&uact=8&ved=0CD

    QQFjAB&url=http%3A%2F%2Fwww.sciencemadness.org%2Ftalk%2Ffiles.php%3Fpid%3D265585%26aid

    %3D21101&ei=iuwlU76DFZHtrQfs24HwAg&usg=AFQjCNEfbJ6HwlmaPYCxiz2wDZCqTRqK-

    Q&bvm=bv.62922401,d.bmk

    Example of commercial firecracker utilizing Chlorate-Sulfur derivatives mix in 1996: Impact Firecrackers

    http://www.privatedata.com/byb/pyro/impactfirecrackers.pdf

    Aware or not; some pyro might not even think twice when priming their Chlorate stars with Black

    Powder, using Black Powder burst charge when using Chlorate stars and also using Black Powder as lift

    charge. Even if using Perchlorate instead, there is still chances that Chlorate impurity inside might react

    even in very small quantity. Because, Perchlorate is produced by further oxidation of Chlorates;

    possibilities of impurity is there.

    Neither way, here I include some of official studies regarding the Chlorate-Sulfur safety issues taken

    from http://www.oocities.org/capecanaveral/campus/5361/chlorate/safety.html

    *Ill just copy everything so that none of the information will be left behind

    *Ill let this open for public discussion as it will be bias if just solely by my point of view which is, I

    already stated that I am not in any position to make any statements. In addition, misleading of personal

    interpretation might likely to happen and some other crucial information is not included either from

    older or modern findings.

  • 11

    Note: This is one long ago study back in the February 1959, in which modern and recent studies would

    be preferred. Even so, this study used as main source of explaining Chlorate-Sulfur instability in other

    related books that cited this experimentation study.

    Chlorate-Sulfur study by Herbert G. Tanner

    Herbert G. Tanner

    Instability of Sulfur-Potassium Chlorate Mixture: A chemical view

    Journal of Chemical Education Vol. 36 No. 2, February 1959

    Numerous amateur rocket enthusiasts suffered serious casualties from

    premature sulfur-chlorate explosions, according to C. Burns (1). This is most

    regrettable. These accidents should challenge elementary, chemistry teachers,

    textbook writers, and civic-minded chemists to do their utmost to teach

    safety to tyro chemists. Chemistry without safety is too frequently fatal.

    The following exposition of the chemistry of sulfur-mixture is presented-with

    the hope that the information will be conveyed to secondary school chemistry

    students as a lesson in safety. Safety is not a series of "'don'ts," but is a

    matter of foresight, with avoidance of hazards. In the discussion of the

    chemistry of sulfur-chlorate mixture, an example of how safety can be

    designed into an experiment is included for the benefit of the chemists of

    tomorrow.

    Sulfur, by itself, is not a particularly reactive element at ambient

    temperatures. Even in the finely divided state it is difficult to ignite.

    Similarly, chlorate is a relatively stable compound at ordinary temperature.

    It decomposes only when heated (2) almost to its melting point of 368'C. It

    is much less reactive at room temperature than is pure oxygen, for example.

    These facts would not incline one to predict that a simple mixture of sulfur

    and chlorate might ignite spontaneously after being stored in a warehouse

    many months, or detonate when a fuse is being stuffed into a rocket charge.

    World accident records for the past, century show that sulfur-chlorate

    stability is erratic and unpredictable. This fact indicates that the mixture

    might contain a concealed chemical trigger. A close look, particularly at

    sulfur, discloses this trigger and the manner in which it becomes cocked.

    There are two basic grades of sulfurcrude and refined. Sulfur produced at

    the mine is called crude sulfur (formerly roll sulfur"). About half of the

    world of sulfur is extracted from the ground in Texas by the Frasch process.

    Traditionally, this raw product is called crude sulfur, even though it has

    the amazing purity of 99.8 to 99.9% sulfur. The chief impurities asphalt

    which is present in the dissolved state. This mere trace of asphalt makes raw

    sulfur difficult to burn on a large scale. Air oxidation at ordinary,

    temperature is detectable only after period of months. Moisture in the air

    assists this slow rusting process.

    Refined sulfur is produced by distillation. The purist is obtained conditions

    that cause the sulfur to condense directly to the solid state, i.e., the

    sulfur is sublimed. The product, called flowers of sulfur, when freshly

    prepared has an average purity of 100.0% sulfur. Even when both grades of

    sulfur are pulverized to the same degree of fineness, flowers of sulfur

    oxidize more rapidly because its surface is cleaner.

  • 12

    Polythionic Acid, the "Trigger"

    Air oxidation probably produces sulfurous acid on the surface of sulfur, but

    this acid has not been detected (3) because, as H. Debus showed, sulfurous

    acid reacts quickly with sulfur to form polythionic acids beginning with

    trithionic acid, H2S306. The latter adds sulfur atoms successively to form

    tetra- and penta- thionic acids. These acids, particularly pentathionic acid

    (5), are responsible for the fungicidal value of dusting sulfurs. Aqueous

    polythionic acids accumulate until the concentration reaches a limit (6)

    where evaporation or a temperature rise will cause partial decomposition

    according to the equation:

    H2S3O6 = H2SO4 + S02 + (n - 2) S

    The reaction is irreversible, but loss of polythionic acids becomes repaired

    by air oxidation of sulfur when the temperature subsides. Reaction (1) is

    significant in that a sudden increase in temperature can, cause a significant

    amount of sulfur dioxide to be formed, not by direct oxidation of sulfur, but

    by decomposition of a concentrated solution of polythionic acids. This event,

    however, must await the formation of a concentrated solution of these acids.

    Reaction (1) is responsible also for the accumulation of sulfuric acid on

    sulfur.The sulfuric acid, being hygroscopic, favors additional production of

    polythionic acids. By capillary action, sulfuric acid coats the surface of

    chlorate and produces chloric acid. Although dilute chloric acid at ambient

    temperature is a very weak oxidizing agent, its presence has given rise to

    the theory that chloric acid is the primary cause of sulfur chlorate

    instability. Sulfur dioxide will react directly with moist chlorate to

    produce chlorine dioxide.

    S02 + 2KC103 = 2CIO2 + K2SO4 (2)

    Chlorine dioxide immediately attacks, sulfur, the chief reaction being,

    2CIO2 + 4S = 2SO2. + S2Cl2 (3)

    Expressing reactions (2.) and (3) as one reaction.

    S02 + 2KClO3 + 4S = 2SO2 + S2Cl2 + K2S04 (4)

    Reaction (4) is a chain reaction because more sulfur dioxide is produced than

    is consumed. Initiation of reaction (4) requires an extraneous source of

    sulfur dioxide. This trigger is cocked by the growth of polythionic acids on

    the sulfur, and is pulled" when the heat from friction, impact, sunshine,

    the like is sufficient to release a threshold amount of sulfur dioxide from

    the "reservoir" of polythionic acids. Heat from reaction (4) quickly ignites

    a portion of the mixture, and, if the gases produced cannot escape readily,

    the mixture will explode.

    Popular formulas for preparing sulfur-chlorate mixtures generally specify

    more sulfur than can be oxidized by the chlorate to sulfur trioxide. The

    reasons for this are not pertinent to this subject, but it is important to

    note that the excess sulfur increases the instability of the mixture by

    favoring formation of a greater amount of polythionic acids.

  • 13

    This trigger" theory was capable of explaining some previously baffling

    industrial accident conditions, but it needed experimental confirmation. It

    predicted that a chlorate mixture prepared with an oxidation resistant crude

    sulfur would be more stable than one prepared with flowers of sulfur.

    Comparative tests were made using ignition temperature as an index of

    stability.

    Experiment A: 2 g of flowers of sulfur, 4 g of reagent grade chlorate, and 4

    g of cleaned and dried sand were intermingled on unglazed paper with a metal

    spatula; 1 ml of water was added dropwise, and the mixing was continued. The

    product was pressed lightly into a thin open-ended cardboard tube made from a

    paper match-cover after the striker strip had been cut off. The tube was laid

    on an asbestos board in an empty ventilated hood and was heated at

    approximately 1oC temperature rise per minute by a heat lamp suspended above

    the tube. The temperature was measured with a thermocouple inserted to the

    center' of the mixture. Ignition temperatures on repeat experiments ranged

    from 82 to 91oC, and averaged 85oC.

    Safety precautions that were designed into the above experiment include

    mixing the powders with a metal spatula and the use of unglazed paper to

    reduce accumulation of static charges. The powder was dampened primarily to

    give it sufficient cohesion to remain in the cardboard tube, but the dampness

    no doubt helped to suppress static charges. The striker strip was removed

    from the match-cover because it contains a sulfide of phosphorus which might

    ignite the mixture prematurely by contact with stray chlorate. Porosity,

    contributed by sand, and the short open-ended tube all owed easy escape of

    gases, thereby reducing the probability of an explosion. Both ends of the

    tube were left open to reduce fire hazard by canceling rocket effects when

    the mixture ignited. Fire hazard was further reduced by the asbestos board

    and by the emptiness of the hood.

    Experiment B: Mixtures similar to those in Experiment A were prepared with

    crude sulfur that had been pulverized until the particles had a mass median

    diameter of 44 microns, thereby approximating the particle size of flowers of

    sulfur. These mixtures ignited, sharply at 124oC. This temperature is above

    the melting point sulfur and indicates that ignition may have been initiated

    by sulfur dioxide produced by air oxidation of hot sulfur vapor.

    Experiments A and B definitely demonstrated the predicated greater stability

    of the crude sulfur mix. However, the chloric acid theory could predict that

    the greater sulfuric acid content of the flowers of sulfur, instead of the

    polythionic acids, would cause the lower ignition temperature. As a matter of

    fact, the flowers of sulfur contained 0.02% "acidity" calculated as sulfuric

    acid. The acidity of the crude sulfur was detectable but was too small to

    titrate.

    As a test of the "chloric acid" theory, Experiment A was repeated using

    flowers of sulfur dampened with sufficient 0.2 N H2SO4 to give it an acidity

    value of 0.50%. When this highly acidified sulfur was mixed with chlorate, an

    abnormal amount of chloric acid must have been formed. In spite of this

    excess, the ignition temperatures averaged only 87oC in close agreement with

    Experiment A. These results dismiss the "chloric acid" theory as a primary

    explanation of instability.

  • 14

    Final confirmation that sulfur dioxide triggers the ignition was obtained by

    repeating Experiment A, but. instead of heating the mixture, a long capillary

    glass tube containing sulfur dioxide flowing at the rate of 0.3 cc per second

    was thrust into the mixture. Ignition occurred almost as quickly as though

    the flame of match had been applied.

    Sulfur--chlorate typifies many fuel-chlorate mixtures. Metallic sulfides and

    polysufides behave qualitatively like sulfur. Phosphorus cannot yield sulfur

    dioxide, but at room temperature it evolves reducing vapors of phosphorus

    oxide and possibly some elemental phosphorus which react so energetically

    with chlorate that an explosion usually occurs before mixing can be

    accomplished.

    Carbon disulfide, rosin, turpentine, thiocyanates, aldehydes, sugars, tannin,

    and numerous other materials that form volatile reducing agents on heating,

    contribute instability to chlorate mixtures. Powdered metals such as oily

    aluminum, zinc, and magnesium are sometimes used with or without other fuels

    in chlorate mixture. These metals are corroded by chlorate. Their chlorates

    are hygroscopic and decompose at relatively low temperatures. The high heats

    of oxidation of these metals could cause local temperatures sufficiently high

    to ignite the mixture. No wonder such concoctions are unpredictable in

    stability.

    Much of the unsavory reputation assigned to chlorate should be reassigned to

    those who have selected the fuels. Apparently availability and cheapness,

    instead of chemistry, have dictated the choice of fuels. Any fuel that is

    subject to air oxidation at ordinary temperature, or forms an unstable

    chlorate, or produces an easily oxidizable vapor below 100oC, or reacts with

    chlorate below 150oC should be excluded. Starch (7) is a fuel that survives

    these requirements.

    Literature Cited

    (1) BURNS, C., J. CHEM. EDUC., 33, 308 (1956).

    (2) BROWN, F. E., AND WHITE, W. C. 0., Proc. Iowa .Acad Sci., 31,291(1924).

    (3) MELLOR, J. W., "Comprehensive Treatise on Inorganic and Physical

    Chemistry," Longmans, Green &, Co., Inc., London, 1947, Vol. 10, pg. S8.

    (4) DEBS. H., Ann.. 244, 76 (1888),

    (5) YOUNG, H.C. AND WILLIAMS ROBERT, Science, 67, 19 (1928)

    (6) MELLOR, J.W. "Modern Inorganic Chemistry," Longmans, Green & Co., Inc.,

    London, 1916, p. 458; EPHRAIM, FRITZ, "Inorganic, Chemistry," Gurney and

    Jackson, London, 1926, p, 463.

    (7) TANNER, H.G. U.S Patnet 1,966,652 (1934)

  • 15

    The main highlighted information from the study

    Lets point out some important information that needs to be taken into account:

    1. Polythionic Acid, the "Trigger"

    2. Air oxidation probably produces sulfurous acid on the surface of sulfur, but this acid has not been detected (3) because, as H. Debus

    showed, sulfurous acid reacts quickly with sulfur to form polythionic

    acids

    3. Aqueous polythionic acids accumulate until the concentration reaches a limit (6) where evaporation or a temperature rise will cause partial

    decomposition

    4. sudden increase in temperature can, cause a significant amount of sulfur dioxide to be formed, not by direct oxidation of sulfur, but by

    decomposition of a concentrated solution of polythionic acids. This

    event, however, must await the formation of a concentrated solution of

    these acids.

    5. This trigger is cocked by the growth of polythionic acids on the sulfur, and is pulled" when the heat from friction, impact, sunshine,

    the like is sufficient to release a threshold amount of sulfur dioxide

    from the "reservoir" of polythionic acids. Heat from reaction (4)

    quickly ignites a portion of the mixture

    6. As a test of the "chloric acid" theory, Experiment A was repeated using flowers of sulfur dampened with sufficient 0.2 N H2SO4 to give it an

    acidity value of 0.50%. When this highly acidified sulfur was mixed

    with chlorate, an abnormal amount of chloric acid must have been

    formed. In spite of this excess, the ignition temperatures averaged

    only 87oC in close agreement with Experiment A. These results dismiss

    the "chloric acid" theory as a primary explanation of instability.

    7. Final confirmation that sulfur dioxide triggers the ignition was obtained by repeating Experiment A, but. instead of heating the

    mixture, a long capillary glass tube containing sulfur dioxide flowing

    at the rate of 0.3 cc per second was thrust into the mixture. Ignition

    occurred almost as quickly as though the flame of match had been

    applied.

  • 16

    The Polythionic acid Trigger mechanism:

    Based on studies conducted by Herbert G. Tenner; February

    Sulfur; S

    Subjected to air oxidation producing Sulfurous acid

    Sulfurous acid + Sulfur Polythionic acid

    Quick reaction as according H. Debus

    If accumulated and form concentrated Polythionic acids

    Concentrated Polythionic acids

    Reservoir

    + Heat decompose into: Sulfuric acid + Sulfur dioxide

    Sulfuric acid; H2SO4

    Favors the production of more Polythionic acid

    Sulfur dioxide; SO2

    Accumulates

    Polythionic acid

    Accumulation reservoir

    Potassium chlorates; KClO3

    Heat released

    Heat supplied

    Heat builds up

    Ignites all sensitive mixtures

    Potassium sulfate; K2SO4

    Sulfur dichloride;

    S2Cl2

    Sulfur dioxide; SO2

    External source

    Sulfur dioxide; SO2

    High acidity level Sulfur; S

    External source

    Sulfuric acid; H2SO4

    Potassium chlorate + acidified Sulfur ignition temperature in range of Experiment A

    = no changes in increasing ignition temperature

    Note: (Heat is supplied)

    Possibilities *on my opinion, it might be

    Sulfuric acid reacts with Chlorate to produce Chloric acid however nothing significant had happen

    Sulfuric acid did not react with Chlorate to form Chloric acid because favor formation on Polythionic acid possibly when reacted with Sulfur *Quick reaction

    Note: The Chlorate-Sulfur mix + Sulfuric acid, it wasnt mentioned that it spontaneously ignited; instead the experiment continues

    The Chloric acid Theory dismissed as primary explanation of instability

  • 17

    Discussion of the Trigger mechanism:

    The main cause of self-ignition is due to the presence of Sulfur dioxide that reacts with Potassium Chlorate which will cause a repetitive chain reaction to cause heat buildup, ultimately cause the ignition.

    However, it wont initiate unless the concentrated Polythionic acid is supplied with heat that promote decomposition to Sulfur dioxide.

    Other notable information:

    The Chlorate-Sulfur mix would not detonate or ignite by itself if mixed.

    Presence of Sulfur dioxide initiate heat buildup; thus cause ignition.

    It is highly sensitive, but not ignited unless external heat is in contact.

    The Chloric Theory is dismissed.

    To initiate the sequence, it requires the Sulfur that oxidized to Sulfurous acid.

    The Sulfurous acid produced; favor the production of Polythionic acid a quick reaction; rather than reacting directly with Chlorates to form Chloric acid.

    The accumulation of Polythionic acid cause the mix to Sour as the acid concentrated.

    The Polythionic acid must be concentrated enough first before able to decompose.

    Concentrated Polythionic acid itself did not cause the ignition.

    The concentrated Polythionic acid did not decompose into Sulfuric acid and Sulfur dioxide unless heat is applied.

    Sulfur dioxide react with Chlorates and gives off heat that ultimately cause ignition.

    In highly acidic condition with introducing of Sulfuric acid did not cause the mix to ignite on contact.

    Sulfuric acid added seems not to react with Chlorate to gives off Chloric acid, or if the Chloric acid was formed; it did not cause the Chlorate-Sulfur mix to ignite. However, it might be different if reacted with the third compound, namely other fuel such as sugar or charcoal which will ignite the mixtures.

    The key to prevent self-ignition:

    Prevent the presence of Sulfur dioxide.

    Prevent the air oxidation of Sulfur to Sulfurous acid.

    Prevent Sulfurous acid to form Polythionic acid to concentrate.

    Prevent unnecessary heat that will cause it to ignite.

    Prevent from in contact with any external source of acids.

    Conclusion: Any mixtures containing Chlorate and Sulfur is highly sensitive to heat, and any other source of ignition; prior to long storage, some oxidized Sulfur will cause Polythionic acid to accumulate and went Sour and might lower its performance and or disrupt with other mixed compounds.

    Question:

    Then, how about the tragic accident in the past happens regarding the Chlorate-Sulfur mixtures? Does that not clear to explain about the mix in which it is highly unstable and prior to self-ignition? Therefore, the question back to the point; what cause the ignition?

  • 18

    Other question rise, and how about if Sulfur air-oxidized in Nitrate-Sulfur Black Powder:

    How exactly solid Sulfur oxidized in air or in moisture as the Sulfur itself generally Hydrophobic (not dissolved in water)?

    In the process of making Nitrate Black Powder, moisture or water is directly introduced. Will this water oxidize Sulfur to Sulfurous acid? And will Sulfurous acid react with Potassium Nitrate to produce Nitric acid in it; thus cause it to ignite?

    It is most likely that the oxidized Sulfur in Nitrate-Sulfur mix will undergo the accumulation of Polythionic acid to concentrate too. This will be just the same.

    If this were true, then if Sulfur dioxide in contact with Nitrate-Sulfur; is this reaction viable? *which is most likely not happen in Nitrate Black Powder? SO2 + 2KNO3 2NO2 + K2SO4 2NO2 + 4S 2SO2 + S2N2 Overall: SO2 + 2KNO3 + 4S 2SO2 + S2N2 Thus, the mechanism of Sulfur Souring or the accumulation of concentered Polythionic acid in Nitrate also can cause ignition.

    And we might conclude that, any mixtures or composition that use Sulfur in it with or without any oxidizer; the Sulfur capable to self Souring or the accumulation of concentered Polythionic acid that can cause further potential ignition.

    *S2N2 or Disulfur dinitrite is decomposing explosively above 30oC which will definitely cause the mix to

    ignite. Explosively of course generate massive heat in general; at insane low temperature above 30oC

    Therefore, Nitrate-Sulfur mix possesses the same degree of danger as Chlorate-Sulfur mix, the difference is; Nitrate-Sulfur mix is less sensitive than that of Chlorate-Sulfur mix. Plus, Sodium Chlorate is known to be more hygroscopic than other oxidizer.

    Possible explanation and more questions arise.

    Maybe in Black Powder, the properties of charcoal fuel itself which is slight alkaline act as anti-acid. This would be desirable to reduce the formation of Sulfurous acid to Polythionic acid until at some point.

    In addition, this would produce another Sulfur-based chemical derived. Will this possibly impart the Black Powder performance? Or will it enhance further? Or will it cause to be unstable? Or just does not affect the powder performance at all?

    For this, we might need to check what would be the source of its alkalinity and possible product from the reaction. Will it gives off or absorb heat during its formation? If sufficient heat is liberated, this would be catastrophic. And the Black Powder itself is not stable, even from a Nitrate based.

    However, in history; Black Powder was been used worldwide in a very long time history. If the concentrated Polythionic acid formation is unstoppable, the Black Powder would turn wet and Sour at significant speed. This lead the powder to have a short shelf life for storage and poor performance; which is might not true as Black Powder have a good shelf life.

    More and more question arise, hence, this subject of Chlorate-Sulfur-fuel issue need further scientific study with solid explanations. The original question is; can Chlorate-Sulfur-charcoal be made into a viable Black Powder? Maybe some Oxidizer-Sulfur-fuel composition is stable, but might not in Chlorate; but how and why? The question is redundant. Back in the history of Chlorate Black Powder which end up in tragedy, same question arise. But today in modern world, sophisticated scientific research can be done. This might prove something valuable in world of pyrotechnic.

    *However, this is just an interpretation made by totally unqualified person in the field of pyrotechnic and or any related; which is me. Therefore, this information cannot be regard as true, as the whole insight might prove to be wrong.

  • 19

    Getting started, getting the right materials and explanations

    In a normal peaceful everyday life, one can purchase the materials locally. Just in case to avoid

    unnecessary attention that might get you in trouble, one should not purchase all the three materials in

    bulk in single store or acting suspiciously. Its obvious and the supplier would know what you are trying

    to do with all those things. Misuse of Chlorate can be charged guilty in certain country. Its printed on

    the label clearly. A wise step is that purchase the materials individually in multiple different store. Lets

    say purchase Chlorate weed killer at Store A. Then, go for another Store B for Sulfur. For charcoal,

    generally everyone buy them. So, this one shouldnt be a problem. Nevertheless, just purchase all the

    required materials in one go. You are the customer. They wont say anything even they knew what

    youre trying to do.

    Different story if in the state of chaos, war and emergency in contrast you might not need the highly

    sensitive Chlorate Black Powder. A military storage bunker would be like a gold mine. Gather your

    comrades and just raid anything that necessary ammunition, firearms, explosives and supplies. Just

    make sure you and your group prepared for the escape route and have the stash house ready and big

    enough for the haul. Its seems like easier said than done (Are you serious?!) In addition to that, use the

    Chlorate to make high explosive instead.

    The best place to find all the materials in one go without any problem would be from the pyrotechnic

    hobby store. One might also consider the online services. Everything that ones might need is there.

    Even Potassium or Sodium nitrate should be available. Thus, please dont even bother on making the

    dangerous Chlorate Black Powder. However, if one still insist and curious to test please be my guest

    although the risk is all yours. The method utilized here also can be used to produce a good useable

    Nitrates Black Powder but not be the best method around.

    The Sodium chlorate

    One can obtain Sodium chlorate from the hardware store under the name of weed killer. Or maybe one

    can also find it at stores that deal with farming supplies. Generally it comes in 1kg per pack. Its primary

    usage in farming is an additive or a booster for the herbicides.

    Check on its label for purity percentage. Some Chlorate weed killer has fire depressant in it that will

    impart the burning rates. 90%+ should be a good enough. However I found one with 99% purity with 1%

    inert impurity as the package states on the label. If one cannot find any that 89%+ pure. One would

    consider to re-crystal the Chlorate salts. Otherwise, another alternative is to construct the Chlorate cells.

    But be sure to get the purest as possible as making manually tend to have high Chlorides impurity in

    which Chlorides in Chlorates has shown to increase the sensitivity with combustible mix.

    Still, purchase the Chlorate would be a better option. Please not to forget to check on the safety

    handling printed on the package label.

    Here I use 99% purity Sodium chlorate as stated on the package not Potassium chlorate. The two

    differences might come into some valuable conclusion out of my known knowledge. Nevertheless,

    obtain the purest possible to avoid high Chlorides content contamination.

  • 20

    Notes and known issues:

    By nature Sodium chlorate is hygroscopic. Thus, it tends to absorb moisture from the surrounding.

    Therefore, keep all the Sodium chlorate based materials in airtight container and store in the dry, cool

    place and out of sunlight reach.

    The Chlorate salt itself is a potential poisonous. Phytotoxic to plants and kills them. It is non-selective

    herbicides thus will harm the surrounding vegetation and plants. Even on the test site where the device

    exploded. The surrounding radius of the exploded individual device known to cause the vegetation and

    plants to wither and literally die which can be seen clearly on the next day. In additional to that, a

    livestock that ate the vegetation might suffer from chlorate poisoning.

    Yet, no known serious health issue when Chlorate solution and its salt to cause specific symptom on the

    skin surface for a momentary being. But its better to prevent with direct contact. However, there might

    be rashes or irritation when the Chlorate dust spread on the skin if prolonged un-washed. When

    Chlorate taken orally or internally, Chlorate poisoning highly possible to occur. Therefore, it is vital to

    acquire info about Sodium chlorate on the net or other source before proceeding. And also, please read

    the warning and other info printed on the purchased Sodium chlorate pack.

    After working with it, there might have too much chlorate dust around. Cleanse yourself by shower and

    change your cloth. Be sure not to inhale the Chlorate dust and or any dust while working. Wearing dust

    mask is highly recommended. However once done be sure to wash the clothing and the dust mask as if

    the Chlorate is presence on the clothing and once it dried can be potential fire hazard when in contact to

    a heat source.

    Warning: Some Chlorate mix cause significant noticeable heat buildup. Once I tried adding Sodium

    chlorate into commercial Flash powder that I took from firecracker. The powder mix liberates significant

    noticeable heat. Thus, avoid such mix. Another study conducted by scientist show that, the presence of

    certain types of Copper compounds as impurity for a Chlorate mix is highly unstable that can cause auto-

    detonation after a few minutes it was mixed; a danger that have far greater chances to happen than

    Chlorate-Sulfur mix. The experiment was repeated and shows the same results. Another incompatibility

    is that Chlorate mix with Ammonium based compound. As such Chlorates with Ammonium nitrate which

    could result in formation of unstable explosive known as Ammonium chlorate. Therefore, avoid Copper

    and Ammonium for Chlorate mix.

  • 21

    The Charcoal

    One can might find charcoal at general store, hardware stores, supermarket and even at hypermarket.

    However, if quality powder you are trying to produce, it is cheaper to make the charcoal yourself. A

    good selection is a softwood types, have low ash contents and the powdered charcoal can be burn easily

    and used up pretty fast. Otherwise, one might find for the softwood Willow charcoal that is used for art

    but will end up being expensive. The activated-charcoal might not be a good choice plus its quite

    expensive I suppose and same goes for the pharmacy grade charcoal.

    The abundant and cheap charcoal would be the BBQ charcoal briquettes. It works but not the best in

    fact its a worst choice for Black Powder. Check the label whether additives is added or not. Such as

    added with quickening agent, petroleum based products, suspicious binder and other impurity should

    be avoided. Starch binder type might be still ok although it should not supposed to have for Black

    Powder making. Some special a little more cost charcoal for grilling might contain un-charred wood to

    meet for their specs for special barbequing. This also should be avoided. Alas, were in desperate

    situation here, dont have enough time to char a wood. Just take it. Take the cheapest one that with no

    additives is preferable.

    If possible, look for air-float charcoal. Its better than the BBQ charcoal briquettes but still might not be

    the best as one might not know of what kinds of wood it is used. Nevertheless, it will work nicely plus it

    is already in a nice powder form.

    For further information regarding on charcoal selection again I suggest the Black Powder Manufacturing,

    Testing & Optimizing by Ian Von Maltitz. Charcoal selection is discussed extensively as because it is the

    most important parts for producing a good useable Black Powder. It also includes list of various specific

    species wood types of charcoal used and the resulting performance it given.

  • 22

    Sulfur

    Sulfur also can be purchased at the hardware store. Other might found one at gardening stores and or

    also at the stores that deal with farming supplies. Generally Sulfur is used to treat the soil. Increase its

    acidity while other uses include as fungicide and also used to fend off crawling creatures for camping

    usage in which the Sulfur powder is spread around the camp site. Sulfur comes in the form of powder

    and chunks.

    The powder form is preferable to be chosen because it is already in powder form. If no other option

    than chunks, reduce it to powder form. Flour of Sulfur would be good enough but Flower of Sulfur might

    be avoided for sensitive mix use. Most Sulfur is pure therefore Sulfur selection would not produce

    significant difference in its performance.

    I got mine in a kilo of package. It is a nice, uniformly dry and clean powder form. When touch the texture

    was like flour completely dry without any slightest moisture. However, Sulfur with moderate and high

    acidity level, moisture and gravel or sand or asphalt should be avoided at all cost as for Sulfur-Chlorates

    this might end up a disaster. Pure, purified and free from acids Sulfur is the better choice for any pyro

    mixes. However, even if it is 100% pure it doesnt mean there is no presence of acids but the least acidic

    possible is preferable. Sand, gravel and asphalt impurity will aid the friction further if friction is issued to

    the powder made plus the powder performance may decrease in burn rates.

    Notes: Once the packs were opened; store them inside an air-tight container, free from moisture and

    heat. This comes with a good reasons to prevent the Sulfur from self oxidizes from open air and

    potential heating while moisture will aid the undesirable process while in storage.

  • 23

    Homemade Chlorate Black Powder process:

    BBQ Charcoal

    Briquette:

    Powdered (mortar pestle)

    Sieved (fine)

    Stored (air-tight)

    Sodium chlorate:

    Powdered (blend)

    Sieved (fine)

    Stored (air-tight)

    Sulfur:

    Already in fine powdered form

    Stored (air-tight)

    Mixing container (Plastic)

    75:15:10 by weight of main materials, dont mind the lumps

    Sealed top, mix intimately slow and gently by turn it around or rotate it sideways.

    Fine Sieve (Plastic)

    Sieve the mixture (fine)

    Crush any lump of remaining materials and force through the sieve

    The remaining powder that could not pass, pour directly into the sieve container

    Transfer back all the mix into the mixing container

    Seal the top; continue mix slowly by turn it around or rotate it sideways until the sieved powder mixture to be evenly homogeneous without any lump presence

    Add about 4% by weight of water

    Stir evenly using a skewer or wooden rod

    Seal the top, mix intimately by slowly rotating around container, and then followed by moderate mixing action (the mix now should be damp but still a little powdery)

    Add more 4% by weight of water

    Again, stir evenly using a skewer or wooden rod

    Seal the top, mix intimately by slowly rotating around container, then followed by moderate mixing action (the mix now should be damp enough, but not wet or watery or not a slurry)

    *if the water were excess, add some dry powder or powder dust from batch before of the same proportion ratio formula until achieve the required dampness, continue mix evenly

    Mortar and pestle

    Damp the interior and top part of the mortar with a little water

    Add the mortar with the damp powder mix half or almost half of the mortar capacity

    Using pestle, pound and knead the mix gently with moderate force.

    Kneading until it becomes a like dough

    Using a spoon, flip the dough, pound and knead it again until it become like dough again stop when consistency is achieved

    Once done, transfer to the temporary air-tight container storage

    Repeat the steps for the remaining damp powder mix

    Temporary container (Plastic)

    Combine all the hard like dough mix into single dough by press them all together.

    The damp mix dough can be stored temporarily until the corning process.

    Corning (Outdoor)

    Bright; not too hot day and clear sky is preferred for the corning process to facilitate the drying

    Take the dough mix and make it into a ball that fit to your palm. *use glove preferred

    Run the dough ball onto the sieve of chosen size with a layer of newspaper below for the damp grains to land, spread the grain evenly

    Let the grain dry under the hot sun, once in a 10-15 minutes use diaper method to flip the grains for evenly drying, re-spread the grains evenly

    Once dried, transfer all the powder to another storage air-tight container for grading

    Grains grading

    Use stacks of layer of multiple sieves of different pore sizes by positioning the smallest at the bottom, moderate at the middle and largest at the top with another suitable container at the very bottom part to collect remaining dusts.

    The larger chunks of grains that did not pass through the top would be crush again gently by breaking them in a tough plastic and sieve again

    At different level, different sizes of Chlorate Black Powder were obtained and can be stored in air-tight container until usage.

    Remaining dust can be re-use for future batch

  • 24

    Notes:

    Always follow general safety rules and keep the working place neat and clean.

    Prevent and avoid any possible source of ignition at all cost.

    Use goggle and mask to prevent dust to get into eyes or respiratory system.

    If using plastic ware, be sure to check and remove any possible static charge.

    If possible, use porcelain or glass substitutes for plastic.

    All the main materials are powdered separately or individually.

    Do not powder Chlorate mixed with other ingredient materials, either Chlorate-Sulfur or Chlorate-Charcoal.

    Weight the ingredient materials using suitable weighing apparatus, example; electronic kitchen balance. For 100g batch; use 75g of Chlorate, 15g of charcoal and 10g of Sulfur.

    Do not overdo the batch, make only adequate batch one at a time.

    Be sure to damp or wet the top and interior part of the mortar, also all of the pestle surface.

    While pounding and kneading, be focus and do not overdo even they were wet. *I am sure there were once I heard a crackling pop sound when I was accidently pounded the mortar sides.

    Be sure the sky clear, bright and warm but not too dry and too hot to conduct the drying.

    Do not leave the drying process unattended. Regularly check for every 10-15 minutes interval.

    It is highly recommended to wear glove or anything similar to prevent direct contact with the wet mass of powder.

    While breaking lager chunks, one can use a pin roller that commonly used for dough making to crush the chunks. Here, using mask is highly recommended as dust will be airborne anywhere. Again, be sure there is no possible source of ignition in the perimeter.

    Store the powder grain in air-tight container; if possible do not open the powder container if not necessary to reduce the air contact.

    Further possible optimization:

    Use better charcoal.

    Mill or ball mill the charcoal.

    Subjected to high pressure press. *Sounds really dangerous for Chlorate!

    Consistence granulation of 4F grade.

    Grading the grains

    Use better method to incorporating the powder.

  • 25

    The makeshift kitchen tissue strip fuse:

    The fuse made by this method is the simplest, fastest, least messy and reliable enough for its purpose.

    The main drawback is that it is hygroscopic and prolonged exposure to open air should be avoided. The

    fuse tend to break if put too much tensile stress on it, slightly moisture and little sugary sticky Chlorate

    for handwork to deal with. In which you have to wash your hand after each fuse paper strip preparation.

    Its looks like it is very messy and tedious to deal with. However, this is the best which I came up with for

    a quick, simple and quite reliable fuse in the time of desperation or just when in need for a fuse.

    To prepare this type of fuse a hot bright day and clear sky is preferred for the drying. If not, the fuse

    wont dry properly as the nature of Chlorate to absorb moisture from the air and the presence of sugar

    will make the drying slower. Preferable time of the day is when around 11.00 A.M when about to get

    into afternoon when the sun shines the best.

    Materials/Apparatus:

    Powdered Sodium Chlorate

    Powdered sugar

    Kitchen paper towel tissue

    Stirrer or a bamboo skewer or any rod non-metal preferred.

    Glass cup or porcelain cup or a plastic container (heat resist)

    Scoop or a washing powder scoop or any other equivalent for the purposes.

    Electric kettle or any to obtain some hot water

    Water resistant glove *optional if you dont want to get contact with the solution directly

    Air-tight container

    Procedure:

    1. Boil some water. Meantime, proceed for the next step.

    2. Take a container as such a cup and pour in 1 parts of powdered Sodium chlorate and 1 parts of

    powdered sugar. And then add up with 2 parts of hot water into the mix.

    Note: The hot water was poured into separate container of cup before take it using the scoop

    and introduced it to the mix. Or just use different scoop of equivalent size for each different

    task. We dont want to contaminate the hot water from the kettle directly. Use common sense.

    3. Stir the mix until all of the powdered chemicals to be dissolved in the solution. If all not just yet

    to dissolve wait 1-2minutes, then continue stirring. It might not all to be dissolved as the

    solution already saturated.

    4. Take the solution in the container outside, fold the kitchen tissue into a rectangular strip and dip

    into the solution.

    5. The wet strip of kitchen tissue with the solution is then let dry under hot bright sun. For faster

    drying, it is better to dry it on a net like surface or if it is drying on a flat surface, after a while

    should flip the tissue once in a while for equal and faster drying.

    6. Repeat the step for remaining solution left with another folded kitchen tissue, dip and dry.

    7. Once all the tissue has dried, take it and put it in the air-tight container and store it in the cool

    and dry place. This is your primary fuse storage.

  • 26

    How to use:

    1. Take out the tissue strip, using a scissor, cut it into a rectangular shape smaller strip with

    desired length. Comply with its width to alter its diameter thickness. If ones need multiple

    number of fuse with the same length and thickness, cut multiple strip of same length and

    width. And store all the smaller pieces in another smaller air-tight container. This is your

    secondary fuse storage. Store back the remaining larger unused portion into your primary

    fuse storage.

    Note: Too small diameter thickness would result a dud fuse. Too big, it will be a waste and

    might not fit to the pass fire hole of your device.

    2. When in need a fuse, simply take out one of the strip from your secondary container and

    roll it into a fuse by folding a little portion at the end of the strip and roll it into a fuse.

    Note: There is no specific procedure for this, but the idea is that just make a roll of fuse from

    the smaller cut strip.

    3. The fuse is now ready to be used and insert to the device pass fire hole.

    Additional notes:

    As mentioned earlier in this section, the fuse itself is hygroscopic. After a while exposed on the open air,

    it tends to wet as it absorb moisture in the air. Therefore, once made into a roll of fuse, have to use it

    immediately or store it back into the air-tight container.

    Always check the burn rates of your fuse. Example, take one of the rolled fuse and cut into lets say 2

    inch length. Take timer, start the timer as you lit the fuse, stop the timer once the 2 inch of fuse done

    burning. Take the time lets say it burns for 12 seconds for the whole 2 inch of it. Thus 12 seconds

    divided with 2 inch we get 6 seconds per inch.

    Warning: Do not use another hazard potential method for drying. As I experienced before, I tried to dry

    it in an electric oven for the lowest temperature possible. The results were tragic. I dont know if other

    method as such using a hair dryer or high watt orange bulb would quicken the drying without cause it to

    ignite. But I think drying it outside would be a better option. However, ones can always experiment

    them. Safety first and use your common sense.

    Notes:

    Before put into use for ignition, take some other piece of the fuse and ignite it. If it can burn at steady rate, the fuse can be used. If not, avoid at all cost and dry them again under the sun.

    The fuse has high probability to be dud and moist at high humidity atmosphere due to the nature of the oxidizer used in making. Use less hygroscopic oxidizer if possible.

    Do not continue to use the same type of the fuse if its dud. Misfire or accidently ignition can occur.

  • 27

    Chlorate-Sulfur mix and Chlorate Black Powder decent sensitivity test

    Accident did occur once in my experience while trying to re-drying the chlorate Black Powder for the 2nd

    time under the bright hot sun, it self-ignite and poofff, 100g of it turned into smoke in a second. Good

    thing I wasnt nearby. At first I suppose it may because the powder was too dry with too many Sulfur

    dust plus high surrounding temperature under the hot bright sun. The Sulfur roles to reduce the ignition

    temperature make it highly combustible in elevated surrounding temperature. Plus, it is mixed with

    Chlorates. But I think thats not the real cause. Its probably because of the static electric charge that

    might be presence on the surface of the drying plastic pan. On one occasion I did notice the static charge

    on the plastic pan that actually makes some of the powder attached to the surface. According to the

    code of practice for the Prevention of Sulfur Fires and Explosion, June 1993; it states that Sulfur has

    excellent electrical insulation properties and under the right condition will readily pickup static

    electricity which if discharged can results in ignition. Therefore, it can be concluded that the static

    charge taken up by the Sulfur in the Chlorate Black Powder dust somehow sparked and ignite the whole

    batch of highly heat sensitive Chlorate Black Powder under the bright hot sun.

    From that day, I never use plastic pan to dry the powder instead I am using old newspaper. Thus, two

    things should be taken into account. One, do not let the drying too long unattended under the bright

    hot sun. And two, careful to not use a plastic-ware that has high affinity to build up static charge and

    always check them before use. This was made with the older method. However newer method yield less

    powder dust. Less dust doesnt mean there is no dust.

    Here the series of test were attempted by means of technically not complete and detail enough to be

    considered as scientific and accurate test due to the lack of proper instrumentation and methodology

    for the intentional purpose of testing. However, I hope these makeshift series of test will be useful

    somehow for further insight and provide general picture on how sensitive this mix is.

  • 28

    The series of sensitivity test:

    Info said Chlorate-Sulfur mix is highly sensitive to heat, sparks and impact. Some said Black Powder also

    sensitive to static electric and the risk of self-ignition. They claim that it is so sensitive just mixing

    Chlorate with Sulfur would result it to cause fire. They said if it has to be mix, use diaper method to mix

    it homogeneously. But experiment show that, it is not soo true for Chlorate-Sulfur as I tested. Such

    sensitivity may be true for Chlorate-Phosphorus mix or the notably the Armstrongs Mix. Instead; an

    explosion is what you get, than just an instantaneous fire. The Armstrongs mix is capable to burn so fast

    to be called detonation on its own, even on the open space. However, I have never tried experimenting

    with the Armstrongs mix just yet. I believe some other enthusiast had already done that and tell the

    tale.

    Chlorate-Sulfur sensitivity test

    I tried to mix the Chlorate Black Powder in 75:15:10 dry mixes all the powdered materials in a common

    plastic container that commonly used for microwave heating. To make it homogeneous, I shake turn it

    around and let the powder mix evenly slowly. Take another container, and pour a small amount of

    mixed powder of around 2-3 spoon into it. Then, I shake it moderately. Nothing happen. I tried to shake

    it for a little while longer moderately and still nothing happen. But of course, if it poses that danger of

    self-ignite, I would not continue to shake it so vigorous like a madman until it catches fire on its own.

    But, the result show that the mix did not ignite if shaken at such moderate force as the claim just mixing

    it could start a fire. Not just yet I suppose?

    Dry impact test

    This time I used 50:50 mixes of Chlorate and Sulfur the most sensitive mix possible. Mix it slowly as

    before in the plastic container; take a very small pinch of the powder onto a piece of metal sheet. I took

    the hammer, and hammer it down. One hit, with slow impact. Nope, it wasnt igniting. After a few

    moderate hit with hammer, bang! It actually explodes with loud bang. I can feel the hammer to kick

    back by the exploding powder. It bangs so loud that my ears rings for several seconds and can feel the

    dizziness. Therefore, the conclusion is it is positive that the mix is impact sensitive.

    How it might works? From my opinion the highly sensitive powder become compressed and at the same

    moment; from the hammer-steel plate impact generate sufficiently enough heat and energy for the

    composition to heat up cause it to auto-ignition and thus exploded.

    In addition, it is best to assume that the Black Powder is also friction sensitive. When storing or loading

    the powder into any container that required being screw, twisting or have threaded lines is be sure to

    clean the threaded lines as such wipe with damp tissue or clean the lines using brush and or tooth brush

    before capping.

    For Black Powder, one would not simply hit the powder with hammer at huge amount right? Or use such

    tremendous force using metal ram rod to ram and pound powder into a casing? By the way, is it that

    necessary? The grains size of Black Powder play important role for a fast powder thus pack it tightly is

    not necessary. Unless one is trying to make a rocket in which this powder is obviously not suitable for

    the job. So, use common sense or better avoid. If such loading is needed, use non-metal tooling and

    always apply pressure gently, slowly and moderately. Never mill all the three main materials dry

  • 29

    especially with Chlorates and Sulfur. If one needs it to be milled or ball milled, mill them separately

    individually.

    Note: wet or damp Chlorate Black Powder doesnt mean that it could not spontaneously ignite.

    Sufficient impact, shock, friction, sparks and heat will cause it to catch fire.

    Spark sensitivity test

    It seems that I learn it on a hard way. For the test, I need a reliable sparks source. I use the used empty

    common gas lighter. It is the one with wheel that produce sparks. I took outside some of the properly

    made Chlorate Black Powder and pour small amount of it onto a brick. As I assume small amount

    wouldnt produce considerable flash when if it ignited. I used lighter sparks to try to ignite it.

    I knew I shouldnt use the sparks so close, as I think small amount wont hurt much. Okay here we go.

    One, two poof! It flashes directly to my fingers. It flashes so fast that I could not take my hand back at

    that instant. The flash was so intense and burns my fingers. Dang! My common sense fails me! The

    burning sensation was excruciating and I have to put my fingers in cold icy water to reduce the pain. The

    pain resides after around a few couple of hours and of course it leaves marks. But it will be healed later

    and most marks will disappear after regenerating. The conclusion, yes it is highly spark sensitive.

    How sensitive is that highly sensitive? Take the dead, empty gas wheel spark lighter; put your finger

    directly on the spot and snap the wheel to produce the sparks. Feel the heat? Its almost undetectable.

    So to put into simpler example, the Chlorate Black Powder spark sensitivity is like a highly flammable gas

    instead it is in solid form.

    However, the actual sparking mechanism might be different than that of direct fire and heating. The

    question is; how does sparks work exactly to ignite them? Is it due to instant increase of high

    temperature spiking in less than milliseconds?

    Static electric charge sensitivity test

    I could not deploy a precise experimentation for it. As Black Powder was generally sensitive to static

    electric sparks therefore I just assume that Chlorate Black Powder would be highly sensitive to static

    charge. Since static charge could not be seen directly, precaution should be taken at utmost priority.

    There is also an issue of some tooling and even cloth would generate static electric by friction. As such

    some plastic containers, plastic bags, PVC made equipment and also synthetic clothing. Therefore, if

    about to use plastic containers, check for the static electric or rub a little the surface before using. Also, I

    think there is anti-static electric spray sold somewhere on the market. That would be a good initiative.

    However do not forget to keep the working place clean and free from Chlorate, Charcoal, Sulfur and

    Black Powder dust as possible and always check for static charge on a possible instrument that might

    build up static charge especially plastics and PVC before using them.

    If using the piezo-electric ignition type it did not ignite. I did test with it before and saw the sparks go

    through the Black Powder in between the source and its end. But maybe I did not test it hard enough

    properly. Just be safe and assume that static electric sparks and the piezo-electric can cause ignition

    thus avoid them at all cost. Note; if piezo-electric actually did ignite them, this source of ignition would

    be very valuable.

  • 30

    I think there were once that I highly suspect it might be that the static electric charge is the cause for the

    sudden self-ignition of the Chlorate Black Powder while drying under the hot sun using plastic pan as I

    stated before at the above section. And I am sure somewhere out there some Black Powder enthusiast

    actually did encounter with this kind of unfortunate static charge phenomenon.

    However to deal with this static charge, in the book Guerillas Arsenal by David Harber, the author

    recommended to ground oneself by using the grounding wire while loading any static sensitive explosive

    filler into the device. It is a length of insulated copper wire in which at one end is looped around one

    wrist, and the other end is attached to the grounded object. With this, it will prevent the static charge

    buildup. There is also a commercial variant for a personal grounding wire for the use of worker that

    works with delicate electronic computer components. Or other approach, wear only cotton cloth while

    working.

    Splinter ember heat test

    Well, in common sense of course it will ignite. But how low the heat required to start the ignition?

    Again, took some of the properly made powder outside. I lit a bamboo skewer splinter then let the fire

    reside until it left with only white ashes with no glowing amber seen directly *some ember is lit under

    the white ashes as I assume. I poke it to the powder and poof! It ignites. Even a very little source of

    ember could ignite it. Thus, the conclusion is that the powder is highly sensitive to heat. Therefore, dont

    even try to heat the powder! Making the Chlorate Black Powder in melting method is absolutely no. And

    dont even think to test or dry the powder in oven with even the lightest temperature.

    In proper instrumentation I assume, the powder would be placed in a closed condition where the

    surrounding temperature elevate in slow progression. Maybe like 10oC per minutes? And record on

    what temperature the powder ignites. For further accuracy it would be repeated several times. This will

    show the true ignition temperature of the powder.

    Storage lifetime

    I store the powder I made into several small plastic bottles and some in small medicinal brown tinted

    glass bottles. In a cool, dry place out of direct sunlight reach. All of the container used to store the

    powder must be air-tight container to prevent moisture and the container must be free from static

    electric. I took some sample and pour it into a small glass transparent glass vial. And put it on the shelf

    out of direct sun light. It stays there for a couple of years with dust and some spider web presence. It

    still in intact. I took some of the powder and ignite it. It still works. There were once I read an article on

    storing homemade Black Powder. One would store it wet in an air-tight container. Only corning and dry

    them when needed. Other stores their dried puck or dried block of Black Powder in an air-tight

    container and only corning them when needed. Of course, keep away from direct sunlight, heat, impact,

    friction, static charge, sparks, acids and any source of possible fire.

    *Medicinal brown tinted glass bottle would be a bad idea for storage if it went wrong somehow, glass

    shards will be threw in every directions. The only bright side it is UV-protected, air tight and less likely

    for the static charge buildup.

  • 31

    Overall Conclusion:

    Overall, from the series of test it can be concluded that the Chlorate Black Powder is highly sensitive to

    heat, impact, friction, static charge, sparks and pre-assumedly acids but it seems it can be stored for

    around couple of years and still works but performance might degrade.

    However one could mix the powder but do not overdo it as such shake or roll it so vigorous which is not

    necessarily needed. Do it gently and keep away from any possible ignition source while handling the

    powder. Despite the violent power it has, it is highly sensitive to compensate and in presence of

    moisture, prolonged storage will cause it to sour or acid build up; thus prolonged storage is not

    recommended and make when only needed, therefore use them in near time. Maybe this is the main

    reasons why Chlorate-Sulfur is highly not recommended as it is unstable and unpredictable in storage,

    plus the nature of Sodium Chlorate is highly hygroscopic. I wonder if Potassium chlorate is used instead,

    because Potassium chlorate is less hygroscopic.

    These are from my point of view. Therefore, it would be a different result if a proper test is conducted

    under proper conditions and instrumentation as scientist usually does for the test. Nevertheless, the

    source of danger should not be pointed solely because of its sensitivity and due to the Chlorate-Sulfur

    mix. The whole process of making Black Powder is a dangerous business. If one is about to make their

    own Black Powder, they should notice the danger beforehand on what they are dealing with.

  • 32

    The typical burn rate test

    Simple method test to determine the rate of burning of a Black Powder is to place them in a line of that evenly contained them. However, this kind of test does not indicate the true potential of the powder burn rate because it has to be confined than just an open burning. And this kind of test is not accurate enough as the test should be exactly the same as in the first it was ignited. Repeated test of the same volume, same weight and the same start timing should be taken into priority to imitate as the same as the first. Repeated results then can be calculated to obtain the average burning rate.

    The method:

    1. Place the powder along the fixed consistent groove line covered the entire volume of the entire length. (make a powder train)

    2. For timing: two common method;

    Hand stopwatch: Start the stop watch as it ignites, and stop when it all burned up.

    Video recorder: Record the burning video, playback; and check the time taken from start igniting to the end of the burning. *Common 30 frame rate per second video recorder would sufficient enough to calculate the time taken.

    3. Repeat the test, but clear the groove first using any suitable tool and once the heat cool down, load next powder train for next run.

    Consistencies that need to be maintain:

    1. The weight or volume of the powder used. 2. The type and the grain of the powder must be of the same. 3. Evenly distribution of powder along the length. 4. Start and stop time measurement (timing). 5. The ambient of surrounding temperature.

    To calculate, simply take the time it need to complete the all the powder, and divide with the length of the powder travel as equal to xxx cm3/second. For


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