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5 Clandestine Production of Methamphetamine

5 Clandestine Production of Methamphetamine

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262



19



Evidence Identification and Collection



Fig. 19.10 The requirement of solutions in the production of many types of illicit drugs makes them a valuable source of definitive proof of

clandestine manufacturing.



Fig. 19.11 The purchase of bulk solvents (left) and pseudoephedrine-containing cold tablets (center and right) by clandestine operators often

initiates clandestine crime investigation.



Pseudoephedrine readily dissolves in alcohol, whereas the insoluble binder (normally starch) usually settles at the bottom

of the container. The alcohol solution is transferred to another container and the solvent is evaporated at room temperature

or on a stove. The recovered pseudoephedrine is collected and further processed in the second step. It is worth noting that

extracting pseudoephedrine from cold tablets using water is also very common.



19.5.2 Manufacturing of Methamphetamine (Step II)

The extracted pseudoephedrine is mixed with hydroiodic acid, red phosphorus, and water in a round-bottomed flask

(Fig. 19.12). This mixture is boiled (“cooked”) for a few hours using a stove or heating mantle. The addition of heat to the

mixture causes the reduction of pseudoephedrine to methamphetamine. It is very important to add water continuously to

prevent boiling to dryness. The absence of water generates phosphine, an extremely toxic gas that is lethal at very low

concentrations.



19.6



Collection of Evidence



263



Fig. 19.12 Large round-bottom flasks and heating mantles are often used in the second step of methamphetamine synthesis (right). Large

container prepared for red phosphorous addition (center); the same container after addition (right). The residual stains are often discovered at

clandestine sites and collected as evidence.



19.5.3 Processing of Methamphetamine (Step III)

Red Devil Lye (NaOH) and an organic solvent, typically Coleman fuel, are added to the solution from step II and mixed

thoroughly. The free base form of methamphetamine is extracted into the organic layer (Coleman fuel) and removed. Table

salt and sulfuric acid are mixed to create a primitive HCl gas generator. The HCl gas is bubbled through the organic layer

converting methamphetamine base into methamphetamine-HCl. The salt form (methamphetamine-HCl) is insoluble in the

organic layer and precipitates out. The recovered methamphetamine is usable at this stage, but its dark physical appearance

is somewhat less appealing to abusers. Therefore, clandestine operators often proceed to the icing stage (Fig. 19.13)



19.5.4 Icing of Methamphetamine (Step IV)

Methamphetamine produced in step III is dissolved in acetone and the mixture is chilled in a refrigerator, producing ice-like

crystals of methamphetamine (Fig. 19.14).



19.6



Collection of Evidence



Definitive proof of at least one step in the Red Phosphorus-HI Method is required to convict clandestine operators. As

expected, the probability of conviction increases dramatically if more steps are proven. Representative evidence collected to

prove various steps is illustrated below:

Samples collected to prove extraction of pseudoephedrine (step I) (Fig. 19.15).

Samples collected to prove methamphetamine production (step II) (Fig. 19.16).

Samples collected to prove processing of methamphetamine (step III) (Fig. 19.17).

Samples collected to prove icing (step IV) (Fig. 19.18).

It is always prudent to collect more than one piece of supporting evidence for a particular step because a single item may

produce negative results upon examination. Evidence collection is the sole responsibility of members of the clandestine

investigation response team. Always remember, clandestine operators have never been exonerated because too much evidence was collected.



264



19



Evidence Identification and Collection



Fig. 19.13 Chemicals used in the third step of methamphetamine synthesis. Red-Devil Lye is a drain cleaner used in clandestine operations as a source

of NaOH (top left). Coleman fuel (top center) is the preferred organic solvent. Methamphetamine-HCl prior to icing (top right) is usable, but lacks the

physical appearance that appeals to most abusers. Common table salt (bottom left) is used to make HCl gas-generators (bottom right).



Fig. 19.14 Methamphetamine

crystals produced after the icing

stage.



19.6



Collection of Evidence



265



Fig. 19.15 Large containers of

white powder are commonly

found at clandestine lab sites.

This type of evidence is collected

to prove stage I of

methamphetamine production

(the extraction of

pseudoephedrine from cold

tablets).



Fig. 19.16 Heating mantles are frequently used as a heat source in the production of methamphetamine. The raw materials are often stored in a

variety of large containers.



Fig. 19.17 Bilayer liquids are

strong evidence of methamphetamine processing. The right

examples are commonly found at

clandestine laboratories and are

collected to prove stage III of

methamphetamine production.



266



19



Evidence Identification and Collection



Fig. 19.18 Examples of

evidence collected to prove the

icing stage of methamphetamine

production.



Fig. 19.19 Remnants of past clandestine operations. The inert nature of water makes it an ideal solvent for recovering residue left in glassware.



19.7



Collection of Washes



In some cases, clandestine laboratories are discovered after the production process has been performed. The inactive site is

generally clean, and very little remains except for a few pieces of empty glassware left behind. Under these circumstances,

fingerprints and washes from the empty glassware are critical in building a case.

The collection of wash is a delicate matter and should be taken seriously. Methanol is generally the solvent of choice

because it dissolves a variety of different substances. Unfortunately, it can also produce chemical changes that alter the natural

pH of the dissolved residue. Subjecting evidence to the possibility of change prior to examination is unacceptable under any

circumstances. If a wash using methanol contains methamphetamine, it can only indicate that the glassware contained methamphetamine. It cannot be stated, beyond a reasonable doubt, that the glassware was used in the manufacturing or processing

of methamphetamine. Therefore, collecting evidence using methanol washes is generally not a sound forensic practice because

it may be disputed during trial.

It is extremely important to maintain the integrity of the clandestine samples prior to testing. To achieve this, water washes

are highly desirable for several reasons (Fig. 19.19). First, the dissolved sample is well preserved with no chemical changes.

Second, water has no affect on the pH of the dissolved residue. Acids and bases are used extensively in methamphetamine

production and their presence can be easily detected in unaltered residues. If, at the time of examination, a water wash is acidic

or basic and contains methamphetamine, the analyst can say, beyond a reasonable doubt, that the glassware was used in the

manufacturing or processing of methamphetamine. Also, fingerprints, if found, can incriminate individual(s) in the clandestine

manufacturing of methamphetamine and add supporting evidence for prosecution.



Suggested Reading



19.8

1.

2.

3.

4.

5.

6.

7.

8.

9.

10.

11.

12.

13.

14.

15.



267



Questions



List four indications of clandestine manufacturing.

List three types of related evidence that supports the existence of clandestine operations.

Explain to members of the jury how the simple observation of a common propane tank indicated illegal activity.

List three solutions commonly found at clandestine sites.

Please explain to members of the jury how the possession of common household items indicates their use in clandestine

manufacturing (hint: quantities).

Outline the steps used in the Red Phosphorus-HI Method.

Why is water addition in Step II critical?

Why is sulfuric acid used in Step III?

What is a common source of NaOH used in methamphetamine production?

What is the purpose of “icing” methamphetamine?

Why is it prudent to collect multiple samples of evidence?

Describe the evidence which is typically collected to prove step IV.

Describe how samples are collected using washing.

Explain to members of the jury why water is preferred over methanol when washing empty glassware.

Why is it generally unacceptable to use methanol as a wash solvent?



Suggested Reading

Christian, D. R. Jr. Forensic Investigation of Clandestine Laboratories; CRC Press: Boca Raton, FL, 2005.

Davenport, T. W.; Allen, A. C.; Cantrell, T. S. Synthetic Reductions in Clandestine Amphetamine and methamphetamine Laboratories: A Review.

Forensic Sci. Int. 1989, 42, 183–199.

Goddard, K. Clandestine Operations. Presented at 37th Semiannual Seminar of the California Association of Criminalists, Newport Beach, CA,

1971.



Examination of Clandestine Evidence



20.1



20



Introduction



The sole purpose of evidence collected from clandestine sites is to prove that operators are engaged in the illegal production

of controlled substances. The discovery of illicit drugs packaged for distribution is clearly compelling evidence, but successful prosecution does not necessarily require the presence of final product at the crime scene. It is quite common to convict

operators using evidence that proves intent to produce and distribute illicit drugs. This broadens the scope of evidence examination to include the following objectives:

Objective 1: Identification of chemicals, solvents, precursors, or elements related to illicit production. The presence of final

product is not required.

Objective 2: Identification of solutions frequently associated with illicit production. The presence of final product is not

required.

Objective 3: Identification of synthetic steps used in illicit production. The presence of final product is critical depending on

which stage is under investigation.

Although the main focus of this chapter is on the Red Phosphorus-HI Method, the science and examination techniques

discussed have applications in the analysis of most drugs and trace evidence. Specific reagents may change or sample preparation techniques may be modified, but the concepts are interchangeable.



20.2

20.2.1



Examination of Evidence to Prove Extraction (Step I) (Fig. 20.1)

Evidence Type



(a) Raw chemicals and bulk solvents.

(b) Glass or plastic containers containing clear or cloudy heterogeneous solutions with solid material settled at bottom. The

solution or solid may be colored depending on the binder used in the tablets. This evidence is an indication of current

clandestine activity.

(c) Moist coffee filters containing a white or colorful residue indicate separation of pseudoephedrine from binder. This

evidence is an indication of current clandestine activity. Dry filters are an indication of past activity.

(d) A coffee grinder with traces of white or colorful solid residue.



J.I. Khan et al., Basic Principles of Forensic Chemistry, DOI 10.1007/978-1-59745-437-7_20,

© Springer Science+Business Media, LLC 2012



269



270



20



Examination of Clandestine Evidence



Fig. 20.1 Summary of clandestine evidence examination to

prove step I.



20.2.2 Examination

1. Test the pH of the solution; it should be neutral.

2. Place a small amount of the solid or liquid sample in two separate test tubes for solubility testing.

3. Add 0.5 ml of chloroform to one test tube and 0.5 ml of water to the other. If the sample mixes in chloroform and water,

the operator used alcohol in the extraction. If the sample is insoluble in chloroform and mixes in water, the operator used

water in the extraction.

4. Evaporate the solvent and perform a base extraction on the solid residue for gas-chromatography mass spectrometry

(GCMS).

5. Perform Chen’s test on the binder, if present. Purple is positive for ephedrine/pseudoephedrine.

6. Perform base extraction in hexane on the binder for identification using GCMS.



20.3



Examination of Evidence to Prove Manufacturing of Methamphetamine (Step II)

(Fig. 20.2)



20.3.1 Evidence Type

Elements: Red phosphorus (P), iodine (I2), sodium (Na), or lithium (Li).

Acids: Hydroiodic acid (HI), hydrochloric acid (HCl), or hypophosphorous acid (H3PO2)

Precursors: Pseudoephedrine

Products: Methamphetamine, amphetamine, N,N-dimethylamphetamine

By-products: Azidridines, substituted naphthalenes, phenyl-2-propanone (P2P), or other transient products.



20.3



Examination of Evidence to Prove Manufacturing of Methamphetamine (Step II)



271



Fig. 20.2 Summary of clandestine evidence examination to prove step II.



20.3.2 Examination

20.3.2.1 Identification of Elements

Forensic laboratories often identify elements using their chemical and physical properties. Confirmatory methods using a

scanning electron microscope are also quite common.

20.3.2.2 Flame-Test for Red Phosphorus

Red phosphorus is the substance that ignites when the tip of a match is rubbed against a course striker. The flame-test is a

confirmatory method used to identify red phosphorus. A small portion of the suspected red solid is placed on a clean glass slide

and exposed to a flame. If the substance is red phosphorus, it will ignite generating a small cloud of white smoke (Fig. 20.3).



272



20



Examination of Clandestine Evidence



Fig. 20.3 Samples of red phosphorus recovered from clandestine crime scenes. The presence of this catalyst is a clear indication of methamphetamine production.



Fig. 20.4 Iodine crystals are found in packaging material that is

discolored by sublimation because iodine containers are often sealed

improperly.



20.3.2.3 Tests for Sodium and Lithium (Nazi Method)

Sodium and lithium are group I metals that react vigorously with water, including water in the air (humidity). Consequently,

they must be stored in an environment devoid of water, often kerosene or any number of thick viscous oils. It is highly likely

that metals recovered from clandestine sites in kerosene (or other oil) are sodium or lithium. For confirmation, a small portion

of suspected metal is placed in a test-tube and water is added. Sodium ignites with a yellow flame and lithium ignites with a

red flame. Unlike most metals, these are relatively soft and can be easily cut with a knife.

20.3.2.4 Identification of Iodine

1. Sublimation: Iodine crystals (I2) characteristically sublime, that is, they convert directly from solid to vapor without

appearing in the liquid phase. The process of sublimation normally taints iodine packaging material yellow (Fig. 20.4).

2. Starch Test: Acidified iodine turns purple when starch is added. Dissolve a few crystals of suspected iodine in 0.25 ml of

acetic acid and add a small amount of starch. The solution turns purple if iodine is present.

3. Chloroform Test: Acidified iodine turns a chloroform layer purple. Dissolve a few crystals of suspected iodine in 0.25 ml

of acetic acid and add 0.25 ml of chloroform. The organic layer (chloroform) will turn purple in the presence of iodine.



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