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MANUFACTURE OF METAMPHETAMINE BY THE "ONE-POT" METHOD

Article · December 2019

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 MANUFACTURE OF METAMPHETAMINE BY THE "ONE-POT" METHOD
KAREL LEHMERT

CBRNe Forensic Sampling Laboratory – VAKOS XT, Prague, Czech Republic

Abstract:

The production of methamphetamine in one container (One Pot Method) has been the dominant
method of production in the USA in the last decade due to strict regulation of precursors, especially
the registration and restriction of drugs containing pseudoephedrine. A similar regime exists in a
number of European countries, so it is possible to expect the method to spread here as well. In order
to verify the available recipes, familiarize yourself with this method for the analysis of possible risks
and obtain comparative material for chemical profiling, a professional workshop focused on specific
types of illegal laboratories was implemented.

Keywords:

Methamphetamine; one pot method; chemical profiling

History of the method

The history of this new method, which is rapidly developing in the world, has been written since 2007,
when the first methamphetamine production plant using this method was secured in the USA. Only 7
years later, it already participates in the production of methamphetamine in the mother country equal
to 98%7. The reason for this extreme increase is the application of legislative restrictions on the
availability of precursors for production by other methods – P2P (uses phenyl-2-propanone and
methylamine), Red-P (reduction of ephedrine using red phosphorus and hydroiodic acid) or the Birch
reduction method. The Combat Methamphetamine Epidemic Act (2005) had a very fundamental
influence on the expansion of the One Pot method, which, by introducing records of the sale of drugs
containing pseudoephedrine and ephedrine with a limit of 9 grams per month, resulted in a rapid
decrease in the number of detected illegal laboratories in the years 2005-7. The massive boom in the
One Pot method has led to an increase in uncovered brews since 20085.

Impacts and risks

Although the method is today the most widespread method of production in the USA, both the
production itself and the by-products are still not chemically characterized in detail. This characteristic
is necessary to determine potential harmful effects on human health and the environment. If we
compare the amount of waste in the production of methamphetamine using iodine technology
(approx. 1 : 30) with the One Pot method (1 : 5-7), there is a certain positive here from an
environmental point of view.
At the same time, the chemical characteristics are also important for the implementation of
decontamination procedures, when the cleaning agents used can react with some intermediate
products and secondary final products to form dangerous or even much more harmful chemical
substances.

The chemicals used in the One Pot method make it possible to work with small amounts of common
substances that cannot be effectively regulated. The simplicity of their acquisition and the
characteristics of the production process, which can take place in its entirety in only one PET bottle,
make this production extremely mobile. In principle, the chemical reaction of the One Pot method is
the same as the Birch reduction, but instead of using ammonia directly, it is developed by reacting
ammonium nitrate and sodium hydroxide in an organic solvent. However, the biggest advantage of the
One Pot method is its minimization – while the most effective Birch reduction method so far needs at
least 30 g of pseudo/ephedrine, the One Pot is enough to effectively carry out the reaction with one
dose of drugs, i.e. 250 mg of pseudo/ephedrine, in 0.5 l PET bottles. This miniaturization enables high
mobility, when the reaction can take place not only in a moving vehicle, but also in a backpack or a
larger bag - and it only takes 2 hours. A number of problems arise from this in the forensic securing of
evidence.

Pic. 1 - Needs for implementing the One Pot method (Source: author)

The extreme increase in the prevalence of the One Pot method in the US is associated with a number
of risks. A number of "chemists" have no idea what they are actually doing and just blindly follow a
recipe from the internet. Since the One Pot method is dependent on the exact order of the individual
precursors, including compliance with the reaction times, many attempts at production using this
simplest method end in chemical or technological failure. This results in the production of unknown
chemical substances, and mainly a large amount of hazardous chemical waste, which is a source of
extreme risk for anyone who will secure or decontaminate this production laboratory.
At this moment, there is no known procedure anywhere in the world to safely decontaminate the
laboratory area after production by the One Pot method. Although the method is relatively the
cleanest of all the known methods of producing methamphetamine, it produces a number of unknown
chemical compounds that it leaves behind in the form of waste. Even the decontamination procedures
published so far (e.g. EPA 2013) are applicable only for some production methods, e.g. Red-P, and their
application to remediation after other production procedures leads to the formation of unknown - and
unmonitored - chemical substances that are equally risky for health as a target product.
Inappropriately used decontamination substances can paradoxically lead to extensive health damage
not only for the remediation staff, but also for the owner or occupants of the property. The personnel
carrying out the remediation often have even less knowledge about the chemical reactions carried out
and the chemical substances used than the "cooks" themselves. There are even opinions published in
low-cost sources5 or at professional conferences (e.g. All Hazards Conference) that the presumptive
idea about the effectiveness of respiratory filters used by security and sanitation personnel when
working in illegal laboratories producing unknown chemical compounds has not yet been fully proven.

Pic. 2 - Initiation of the reaction in the vessel (Source: author)

Pic. 3 - Defective development of a chemical reaction (Source: author)

Theory of production

There are a number of practical implementations of the One Pot method1, 2, 3, 4, 6, 8, 9, 10. The following
chemical reactions are carried out simultaneously in one reaction vessel:

- the reaction of ammonium nitrate (NH4NO3) with sodium hydroxide (NaOH) produces ammonia

- reduction reaction through some alkali metal, releasing an electron into the reaction solution

- organic diluent with dissolved pseudoephedrine/ephedrine, which is reduced to methamphetamine

as the recipient of the released electron

A number of recipes are freely available on the Internet. But as with everything else, there are mistakes
here too, which will bring at least a number of complications to an uninstructed person interested in
their implementation. A typical street implementation obtains chemical substances in various
improvised ways depending on the legislative conditions of a specific country. Ammonium nitrate can
be purchased both in analytical purity and in technical quality, as it is used as an effective nitrogen
fertilizer in agriculture or to disinfect pool water. It is monitored as a precursor to explosives, the
purchase and possession of which is prohibited to non-business natural persons without a permit in
accordance with Regulation EP/RE No. 98/2013. Together with sodium hydroxide, there is a rapid
evolution of gaseous ammonia, increasing the internal excess pressure, often up to the destructive
pressure of the working vessel.

The reaction takes place in an organic solvent environment. In the United States, camping stove fuel
(eg Coleman Camp Fuel, kerosene, etc.) is most commonly used at street level, while in Europe the
availability of organic solvents (cyclohexane, diethyl ether, etc.) is significantly easier. The reduction
reaction is mediated by an alkali metal in the presence of water. At the same time, the reaction is
strongly exothermic, additionally producing hydrogen gas. The necessary alkali metal is obtained in
improvised conditions, e.g. by extraction from lithium batteries. A big difference, compared to
traditional high-volume productions, is the production method, where instead of increasing the
volume of reaction vessels, manufacturers proceed by multiplying them into a series. The discovery of
a vehicle with a large number of PET bottles scattered in the interior is no exception.

Pic. 4 - Reaction vessel after the end of the production process (Source: author)

Here is the basic risk of the entire production process. The pressure of the reaction gases exceeds 7
bar – that is 2x more than in a bottle of sparkling wine, which represents a significant risk factor with
the recorded volumes of the reaction vessels (even more than 20 liters). At this pressure, gaseous
ammonia already liquefies and is the basis of the entire reaction. Overpressure of hydrogen gas can
lead to a rupture of the wall of the reaction vessel and an explosion accompanied by splashing of liquid
with pH=14. The second, no less significant danger is the alkali metal itself. If it is not ground into really
small particles, then it very often sticks to the wall of the reaction vessel. The increasing temperature
during the reaction with water can lead to melting of the wall of the reaction container (e.g. PET
bottles). The author witnessed an accident where the reaction gas drove an organic diluent under
pressure through a hole melted in the wall of a plastic bottle. The subsequent ignition of the diluent
by a spark from a piece of lithium was surprising even to trained personnel. Lessons learned show the
necessity of occasional shaking of the reaction vessel to prevent lithium chunks from sticking to the
wall of the reaction vessel.

Pic. 5 - Ignition of the reaction mixture (Source: J. Wagner)

At the end of the reaction time, it is necessary to filter the contents of the reaction vessel through filter
paper (typically a coffee filter), where the filtrate with a high content of methamphetamine is
subsequently processed by "salting out" the methamphetamine hydrochloride with hydrogen chloride
gas developed in a separate vessel using sulfuric acid and sodium chloride. Alternatively, acid is also
used directly - hydrochloric for hydrochloride, sulfuric to obtain methamphetamine sulphate.
Precipitation of the methamphetamine salt is visible. Subsequently, the precipitate is filtered again
and can be processed by recrystallization according to the required crystal size. The result is a product
with a purity of 95% and a yield of 78% according to available internet recipes for production by this
method.

Pic. 6 - Preparation for chemical profiling (Source: author)

Practical production demonstration

In the framework of the workshop "Clandestine Laboratory and Remediation" realized by the author
as part of the concurrence of research projects in cooperation with the specialists of the British SCJS
for the staff of the Turkish Kriminal Daire Başkanlığ (KDB) in Ankara, Turkey, the preparation of five
experimental boils by the One Pot method was carried out with the aim of characterizing the product
for future needs forensic typing. The tablet containing pseudoephedrine was secured by direct
purchase of the drug at a local pharmacy, where unlimited purchases of up to 25 mg of
pseudoephedrine per tablet are possible. Other necessary components were purchased partly in the
retail network, partly from the institute's stock. For the test boil, a small volume of the reaction vessel
(500 ml PET) and a 1:1 ratio of precursor to organic diluent were chosen for the safety of the
participants.

The participants were instructed about safety rules and possible risks, familiarized with the work
procedure, each work group received precursor weights, tools for lithium extraction and a reaction
vessel. With safety in mind, the test boil was carried out outside near the fire pit with a prepared
emergency nest consisting of a water bath for emergency cooling of reaction vessels, a FirChem fire
cape, BlankFir fire blanket and a snow extinguisher. All participants and teaching staff were equipped
with personal protective equipment.

Each group processed their own boil according to a common procedure. Already during the
preparation, the differences became apparent, when one of the groups did not use the entire amount
of weighed chemicals and another incorrectly identified the lithium layer in the disassembled battery.
An ordinary PET bottle with a screw cap without additional modifications was used as a reaction
container. After the preparations were completed, two reaction vessels (Nos. 1, 2) were left in their
original state without the addition of water, three reaction vessels (Nos. 3-5) received the addition of
water. Overpressure was released in reaction vessel No. 1 in 20 min. In 45 min, reaction vessel No. 2
burst with a microcrack at the bottom. A quick transfer to a water bath cooled her down and slightly
reduced ammonia emissions into the environment. After the end of the reaction, the water bath had
pH=14. The constant presence of an operator, shaking the reaction vessel, was shown to be necessary
in order to prevent lithium pieces from sticking to the wall of the reaction vessel and at the same time
for the reaction to take place correctly in the entire volume of the tablet.

Pic. 7 - Reaction waste (tablet material) with lithium residues (Source: author)
When the time limit expired, the reaction containers were handed over for evaluation, when the
reaction in container No. 1 no longer visually proceeded properly (non-homogeneous distribution of
the tablet substance in the solid phase), container No. 2 showed similar deficiencies in addition with
apparently insufficient pressure of the reaction gases, containers Nos. 3 and 4 were optimally
pressurized with the correct colouring of both the solid and liquid phases, in container No. 5 the
reaction did not proceed properly due to the minimal amount of lithium.

Pic. 8 - Working solutions with different colour products (Source: author)

Then the individual groups took the reaction vessels to the laboratory, where they were to prepare
them by finalizing them in a fume hood for analysis. Workgroup No. 3 did not properly decompress
the reaction vessel, and the subsequent explosive decompression contaminated the entire hood area.
The pressure of the explosion threw the operator away from the hood. The other groups learned their
lessons and worked more cautiously. The gas pressure measurement in the reaction vessel showed a
value exceeding the gauge's working range of 7 bar. After filtering the solutions, the individual products
were tested for the presence of methamphetamine using the Herosol test (Mistral Inc.) with a positive
result for products #1-4. Methamphetamine hydrochloride was precipitated from the working
solutions by titration of the filtrate with hydrochloric acid. Although the same starting materials were
used for all solutions, the result was four different product colours for the four groups, ranging from
white to yellow and orange to pink.
Pic. 9 - Product crystalline and amorphous (Source: author)

Crystallization gave, in addition to white crystals, a pink amorphous mass. Analysis by infrared
spectrometry (FT-IR) and gas chromatography (GS/MS) showed the presence of methamphetamine
and ibuprofenate, but no trace of residual pseudoephedrine was found. An interesting finding was the
effect of trace amounts of reactants on the yield, when these rapidly increased the purity and yield of
the entire reaction. Unidentified peaks of other organic compounds occurred near both known
compounds.

Pic. 10 - Analysis of yield sample #2 (Source: Richard Hooker, SCJS)

Taking into account the history of health problems of laboratory workers suspected of chronic
intoxication with psychoactive substances, swabs from the laboratory equipment were taken and
subsequently analysed in the laboratory area. The results of the analysis showed spatially extensive
contamination of clean analytical spaces with methamphetamine and heroin, including additional
substances (paracetamol, caffeine).
Pic. 11 - Wall swab (Source: Richard Hooker, SCJS)

Pic. 12 - Furniture swab (Source: Richard Hooker, SCJS)

The experiment verified the simplicity of the production process, which, despite the apparent
simplicity, may not lead to a successful end. The result, which differs in appearance and structure
despite the same input raw materials, turned out to be interesting. This, together with miniaturization,
short preparation time and material minimization, presents a great challenge for detection and proof.

From the safety point of view, the most important risk points of the production process were
manifested - the increase in pressure during the reaction and the exothermic nature of the reaction.
The amateur approach of small-scale manufacturers can lead to unexpected emergency situations,
including fires or burns (eyes, respiratory tract, skin). For untrained safety personnel who do not
recognize the reaction vessel correctly and in time, the moment when they try to open an unknown
vessel is a source of major risk. A momentary decompression of a strongly alkaline solution under a
pressure of 7 bars can deprive a person not only of his sight.

An unexpected result was brought by the analyses of smears of laboratory furniture in clean rooms,
which showed massive contamination with processed substances even in places where only pre-
prepared samples are already received. The spread of fine aerosol throughout the interior is not only
a risk from the point of view of process quality, but also from a health point of view for the staff.
Conclusion

In conclusion, one can only hope that even though this production procedure has not yet been
experienced in our country, it will not become fatal for someone. Because there is a lot of potential for
injury during the securing of physical evidence in this method of producing methamphetamine. The
appearance of the reaction vessel is not unified, but there is always a common denominator – a high
internal overpressure of a highly corrosive liquid. Risky technology also becomes a secondary source
of risk, when a Class I combustible is found in one container together with a source of open fire in the
form of lithium and water. There are a number of documented cases where the reaction vessel was
ignited due to careless handling by the manufacturer or during an attempt to get rid of evidentiary
material during the inspection of luggage or a motor vehicle. In general, it can be said that from a
criminological point of view, this method is poor in terms of evidence. Precursors are freely available
and unregulated, except for the drug that serves as the source of pseudoephedrine. Technological
means belong to commonly occurring material. Until the moment of drying the final salts of
methamphetamine, the producer does not come into contact with anything that would leave
demonstrable traces of illegal activity. A significant negative is also the speed and complexity of the
reaction, which shortens the reaction time for securing evidential material. The entire method is
relatively the cleanest from a hygienic point of view compared to other production methods. But that's
the only positive thing that can be said about her.

Experience from practical production shows that, in the future, great care will be required when
inspecting and transporting unknown containers, because the reaction container does not show at first
glance what danger it hides. Even an ordinary PET bottle thrown on the floor of a car can be a risk. And
even with early detection, careless transport is enough to cause an accident. All of this can be helped
by good theoretical preparation and knowledge of correct handling procedures, including possible
risks.

Literature:

1. Abdullah, S. A.: One‐Pot (Shake & Bake) Methamphetamine Labs: Presentation. 2013, online z
https://www.scribd.com/document/168980897/DWorley-OnePot-3
2. Angelov, K.: Methamphetamine. 2013, online z
https://www.scribd.com/document/120642722/methamphetamine
3. Bennett, S.: Shake and Bake 1. 2011, online z https://www.scribd.com/doc/62027279/Shake-
and-Bake-1
4. Candyman3988: Shake & Bake. 2011, online z https://www.scribd.com/doc/75489753/Shake-
Bake
5. Ciesielski, A. L.: Characterization of Clandestine One Pot Methamphetamine Laboratories Using
Gas Chromatography-Mass Spectrometry and Liquid Chromatography-Tandem Mass
Spectrometry. Oklahoma State University, Stillwater, 2017
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experiment
10. s.1232: Uncle Fester´s Nazi Methamphetamine Table Top Recipe. 2008, online z
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Dedication
Findings presented here are results of research funded by the Ministry of Industy CR (grant no. FV TRIO
30483 „Minimalization of Health Effects of Residual Contamination After Illicit Narcotic Production“)
and EU (grant no. TR 16 IPA JH 02 18 „Strengthening the Capacity of Turkish Forensic Laboratories in
Combating Illicit Drug Trafficking“).

Corresponding author:
Karel Lehmert, e-mail: lehmert@cbrn.cz
CBRNe Forensic Sampling Laboratory – VAKOS XT, Pernerova 28a, 186 00 Praha

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