Journal of Clandestine Laboratory Investigating Chemists Association

Abstracts from the publication Journal of Clandestine Laboratory Investigating Chemists Association

An Unsuccessful Clandestine Synthesis Of Amphetamine
Sanford A. Angelos and Jack K. Raney, United States Drug Enforcement Administration, North Central Laboratory, 610 South Canal Street, Chicago, IL 60607

Two clandestine amphetamine laboratories produced a number of samples containing phenylacetic acid and alpha-phenylacetamide. From the chemicals found at the laboratory site, the most likely procedure should have been to first manufacture phenyl2propanone and further produce amphetamine. What became suspect from the analysis of the mixture was that the clandestine laboratory operators had attempted to carry out the synthesis of both phenyl2propanone and amphetamine in the same reaction. The results were that an impurity, alpha-phenylacetamide, usually found in small amounts was now the major product of the reaction. Spectral data of the various samples seized are presented.

The Use of Chemical lonization-MS in Analyzing Novel Amphetamine Reaction Mixtures
Richard R. Laing; Health Canada, Health Protection Branch, 3155 Willingdon Green, Burnaby, BC V5G4P2

In a recent Clandestine lab seizure in Vancouver, B.C. (28/06/93) the cook stated that he was cooking a “legal” nonscheduled amphetamine analogue. Since a preliminary examination of some of the seized exhibits was negative, Chemical lonization-MS was examined using 7 amphetamine-like compounds to determine its applicability in singling out an amphetamine analogue from a complex reaction mixture.

Examination of MDA
V. Sorokin, A. Beljaev, K. Ponkratov; Criminalistics Center Ministry of Internal Affairs of Russia, 123060, Moscow, Raspletina Street, 22, Moscow 123069

Illegal manufacture of 3,4-methylenedioxyamphetamine (MDA) has been organized at pharmaceutical plant in Oljane town (Latvia) in the late 1992. Isosafrole has been oxidized with formic acid and hydrogen peroxide mixture. Product of this reaction has been hydrogenized with an ammonia and gaseous hydrogen mixture in methanol media (pressure 1.5 MPa; catalyst Ni-Rainey has been used). In result of this reaction MDA has been obtained. Finale product has been produced as white tablets. Tablet’s weight is about 300 mg. Investigation with employment TLC, GC and IRFT methods after purification of the probe by means of a solid-phase extraction made it possible to identify MDA.

“Clandestine Drug Lab Chemistry Illustrated
Jeffrey R. Dovci, Oregon State Police Crime Lab, 650 Royal Avenue Suite 12, Medford, OR 97504

Clandestine drug chemistry is complex and presents an intellectual challenge even to the trained forensic chemist. Providing expert testimony on the subject can prove to be an even greater challenge. To effectively testify to any scientific principle or conclusion in a court of law, it is often necessary to assume the role of educator. The expert must adequately instill a functional level of technical understanding in the minds of the judge and jury so they may fully comprehend the significance of the expert’s opinion. If the expert fails in this task, even the most insightful presentation will fall on deaf ears and its relevance will be lost. As an educator, the expert must utilize any tool at their disposal. One of the most valuable tools the expert can use is visual aids. Visual aids can be in a variety of formats including slides, overheads transparencies, and poster graphics. The following computer generated and hand painted illustrations are examples of visual aids which have been used successfully in both the state and federal courts of California and Oregon. The computer graphics were generated on a 486/50 MHz personal computer equipped with 8 MB of RAM. The system includes a 170 MB IDE hard disk and a super VGA non-interlaced monitor with a BOCA 1 MB video card. The software used was Computer Support Corporation’s “Arts & Letters” with Windows 3.1. The color illustrations were generated on a Hewlett – Packard DeskJet 500C inkjet printer.

Mope Dope and AIDS Cures: Central California Drug Lab Scenes, 1992-1993
Jerry Massetti; California State Department of Justice, Fresno Regional Laboratory, 6014 North Cedar Avenue, Fresno, CA 93710

Two new distinctive types of clandestine drug laboratories have been observed in Central California during the last year. The first was a highly stylized, repetitive organized crime type of operation which used the hydriodic acid/red phosphorous reduction of ephedrine to methamphetamine. This reaction has been used in Central California for years; however, some innovative variations have streamlined the process. One of the scenes corroborated rumors about multiple tons of ephedrine being processed in this way. The repetitive aspect of these labs constitute an interesting study in linking sites of serial crimes with physical evidence. The second kind of lab newly observed in Central California in the past year produced hypercin from St. John’s Wort. AIDS cures have occurred in other clandestine drug laboratory investigations in California.

Clandestine Aminorex, A Designer Drug Parent Finds the East Coast
Jason W. Freed, BS, and Vincent Cordova, BA; National Medical Services, Inc., 2300 Stratford Avenue, Willow Grove, PA 19090

In this presentation we describe a case of a fragrance laboratory being used as a cover for clandestine d,l-aminorex laboratory. The peculiar twist of this case was that d,l-aminorex is the parent compound of the more conventionally recovered 4-methylaminorex, a federally controlled Schedule 1 drug. Additionally, d,l-aminorex was not, at the time, a common street drug in the Philadelphia or surrounding east coast area. Work with undercover officers throughout a lengthy investigation enabled a search and seizure of the laboratory. Findings from street purchases and samples from the lab identified d,l-aminorex. Precursors identified from the laboratory consisted of dl-2-aminolphenylethanol, cyanogen bromide, various solvents, and sodium acetate. These findings led to the confiscation and dismantling of the laboratory and to the arrest of the suspect involved in producing the d,l-aminorex.

Disposal Technologies
Jeffrey L. Buntrock and Robert E. Brown; Chemical Waste Management, Inc., 4227 Technology Drive, Fremont, CA 94538

In 1976, the Resource Conservation and Recovery Act, or RCRA, became law. This was the first effort on the part of the Federal Government to regulate the management and disposal of hazardous waste, and was comprehensive and far-reaching in its impact. Since then, RCRA has been amended several times, with the 1984 Hazardous Solid Waste Amendments, or HSWA, being of the greatest significance. These amendments to RCRA have, with few exceptions, eliminated the disposal of hazardous waste directly into landfills without previous treatment to specific standards. Management and disposal have been further complicated by State requirements, and the necessary inclusion of materials previously unregulated by the Federal Government. Finally, with regards to clandestine drug wastes, regulatory requirements extend from RCRA (Resource Conservation and Recovery Act), TSCA (Toxic Substances Control Act), State Programs, and even some pressures from the NRC (Nuclear Regulatory Commission) for management of low-level radioactive materials. This presentation discusses the management and disposal options and opportunities in the 1990’s. Included is an overview of the waste streams typical of Clandestine Lab Sites, and the available treatment technologies for each. Specific discussion will include examples of disposal facilities of each type, as well as possible alternatives. The presentation endeavors to provide an overview of hazardous waste management and disposal as it pertains to Clandestine Drug Lab materials.

Fatalities Resulting From Clandestine Drug Manufacturing Laboratories
Roger A. Ely, Drug Enforcement Administration, Western Laboratory, 390 Main Street Room 700, San Francisco, CA 94105; and Steven B. Johnson, Los Angeles Police Department Crime Lab, 555 Ramirez Space #270, Los Angeles, CA 90012

Clandestine drug laboratories are known to contain extremely hazardous chemicals which can cause serious injury or death to the lab operator and to the investigator. Fire and explosion from organic solvents and reactive materials remain a serious threat. One illicit synthetic method to methamphetamine using a red phosphorus – hydriodic acid reduction of ephedrine can be especially dangerous due to the reactants and byproducts formed from their reaction. Two separate incidents resulting in the deaths of three people in Los Angeles, CA, and two in Post Falls, ID, will be presented with crime scene reconstructions and postmortem findings.

Methamphetamine Synthesis Via Reductive Alkylation Hydrogenolysis of Phenyl-2-Propanone with N-Benzylmethylamine
Harry F. Skinner; Drug Enforcement Administration, Southwest Laboratory, 410 West 35th Street, National City, CA 91950

Methamphetamine was synthesized by reductive alkylation hydrogenolysis of phenyl-2-propanone with N-benzylmethylamine. The expected product N-benzylmethamphetamine, once formed, undergoes hydrogenolysis to methamphetamine and toluene. The progress of the reaction, the intermediates formed during the reaction, and the products were analyzed by gas chromatography and mass spectrometry.

Examinations of Duct Tape in Clandestine Labs
Max Courtney; Forensic Consultant Services, P.0. Box 11668, Fort Worth, TX 76110

In case after case involving clandestine amphetamine or methamphetamine laboratories, the violators have been seen to employ duct tape. Common examples of its use include taping glass joints and sealing of packages of product or boxes of equipment. Numerous class characteristics and individual characteristics are discussed in this application of criminalistics to the drug enforcement area. Duct tape offers a wealth of information in comparing questioned and known samples for tying a violator to an offense.

Cocaine in Bleach: Destroying the Evidence.  Identification of Degradation Products
Alexis Carpenter and Richard R. Laing, Health Protection Branch, Drug Analytical Service, Health Canada, 3155 Willingdon Green, Burnaby, B.C., V5G 4P2

In recent months, this laboratory has received over forty unusual exhibits from Edmonton, Alberta. These exhibits were found to contain liquid bleach, some of which had traces of cocaine. The samples were seized during raids on fortified shooting galleries where buckets containing bleach (typically one-gallon ice cream containers) were found. It was suspected that the occupants had dumped quantities of cocaine into the bleach for the purpose of destroying the evidence. We were able to identify cocaine in some of the samples, but in many others cocaine was totally absent. Closer inspection of GC-MS data revealed several compounds present in large quantities and appeared to be related to cocaine. These compounds were identified as degradation products with norcocaine and N-formylcocaine being the most predominant.

The Analytical Profiling of Methamphetamine of Various Origins
Peter Fifka, Jiri Zapletal, and Jaromir Novak, Police Institute of Criminalistics, 9.Maja 1, Banska Bystrica, Slovakia, 97486

Methamphetamine hydrochloride salt has been prepared by two different syntheses:

The reductive amination from 1-phenyl-2-propanone and methylamine; and

The reduction of ephedrine using iodine and red phosphorus.

Prepared samples were examined after previous preconcentration of impurities by GC-MS analysis. Some compounds were identified among the impurities. Chromatographic spectra of both are different and by the presence of some specific impurities, it is possible to determine the way of the synthesis.

Sodium Bicarbonate Assay in Controlled Substance Exhibits
Thomas R. Ekis and Max Courtney, Forensic Consultant Services, PO Box 11668, Fort Worth, TX 76110

Controlled substance samples occasionally are encountered wherein sodium bicarbonate also is detected, especially in phenethylamines and cocaine. Synthesis strategies seem to suggest no logical reason for the presence of bicarbonates in phenethylamines beyond its use as a cutting agent; there is no apparent way to determine whether its presence in “crack” is as an intended cutting agent or as a remnant from the preparation of the cocaine free base. For either legal or investigative reasons, assay of the sodium bicarbonate is sometimes required. Due to the buffering properties of the bicarbonate ion, volumetric analysis can be difficult. This presentation deals with the methodology of titration and the selection of proper endpoint indicators suitable for titration of bicarbonates.

The Domestic Chemical Diversion Control Act of 1993
Clyde F. Richardson, Drug Enforcement Administration, Diversion Control Section, 600 Army-Navy Drive, Arlington, VA, 22202

This presentation will explain the provisions of the federal Domestic Chemical Diversion Control Act of 1993 which became effective on April 16, 1994. The new law enhances DEA’s ability to regulate the distribution of certain chemicals used in the illicit manufacture of controlled substances. It places more requirements on handlers of these chemicals, provides administrative authority for regulating drug products containing ingredients used in illicit manufacturing, and places reporting requirements for manufacturers of regulated chemicals.

The Ritter Reaction Using Safrole: An Encounter In Two Clandestine Labs
Richard R. Laing and Brian Dawson, Health Protection Branch, Drug Analytical Service, Health Canada, 3155 Willingdon Green, Burnaby, B.C., V5G 4P2

In two recent MDA clandestine lab seizures, references were found relating to the Ritter reaction in which safrole, acetonitrile and concentrated sulphuric acid are reacted together at cold temperatures. In repeating the synthesis the desired intermediate N-acetyl MDA was not found at any stage of the reaction. The major reaction product, although seeming to relate to MDA was partially characterized using IR spectroscopy and mass spectrometry but require 1H and 13C NMR techniques for structure confirmation. The major product 3,4-dihydro-1,3-dimethyl-6,7-methylenedioxyisoquinoline does not appear to be the desired end product and has also recently been identified in two street samples from the Vancouver area.

MDA From Safrole by the Ritter Reaction
R. Kazlauskas and V. Murtaugh, Australian Government Analytical Laboratory, PO Box 385, Pymble, Sydney, NSW, Australia, 2071

The underground book by Uncle Fester, “Secrets of Methamphetamine Manufacture,” mentions use of the Ritter reaction to make MDA from safrole, by analogy to making amphetamine from allybenzene. But when the reaction is applied to safrole and acetonitrile, it gives only a low yield of the expected product, N-acetyl MDA. The major product appears to be an isoquinoline. It is suggested that clandestine lab chemists can use this compound as an indicator of the Ritter or related reactions.

The Use of Hydrogen Peroxide in Ephedrine Reductions: A Growing Trend
Tim McKibben and Troy Ward, Aurora Police Department, 15001 E. Alameda, Aurora, CO, 80012; and Dawn Sorenson, San Bernardino County Sheriff’s Crime Laboratory, PO Box 569, San Bernardino, CA, 92402-0569

The use of hydrogen peroxide in the reduction of ephedrine to methamphetamine has become popular in several western states. The use of this reagent introduces several new possible reaction and byproducts. The use of peroxide should also be a cause of concern because of its explosive properties. This paper will introduce the use of hydrogen peroxide, its possible side reactions, byproducts, and impurities to the forensic chemist.

An Overview of Central California Clandestine Methamphetamine Laboratories Associated with Mexican Nationals
Jerry Massetti, CA Department of Justice Regional Laboratory, 1704 East Bullard Avenue, Fresno, CA 93710

Large capacity clandestine methamphetamine laboratories associated with operatives from Mexico continue to inundate Central California with increasing frequency. Work crews report to remote, secluded, usually agricultural sites to discretely deliver, process, and dispose of chemicals and equipment used to manufacture methamphetamine. Seven and ten ton shipments of ephedrine have been documented. Some manufacturing incidents have aroused environmental impact concerns. An overview of recent cases will be presented.

Application of the SplitPeaTM FT-IR Micro Sampling ATR Apparatus in Analysis of Drugs of Abuse
Richard R. Laing, Health Protection Branch, Health Canada, 3155 Willingdon Green, Burnaby, BC, Canada V5G 4P2

The SplitPeaTM (Harrick Scientific Corporation, Ossing, NY) is an Attenuated Total Reflectance (ATR) experiment module consisting of a purgable condenser optics and an external sampling stage for most FT-IR Spectrometers (Nicolet Magna 550, Madison, WI). Either ATR or Diffuse Reflectance (DR) can be selected by simply changing the sample holder. While ATR is primarily used for surface analysis such as films, fibers, and pastes the SplitPeaTM in DR mode affords a wider application and has been applied to routine drug analyses in our laboratory. The external sample stage allows facile placement of the sample on the contact surface at the optics focus giving excellent spectra. Powders such as cutting agents or methamphetamine can easily be run neat without the preparation of KBr disks in ATR mode. Extracts such as LSD base can be spotted directly on the 350-300 micron Si crystal for ATR or on the traditional AgCl disk in the DR mode. Films and residues on a variety of surfaces can also be analyzed which normally using traditional IR techniques would be very difficult.

Estimation of Drug Product Yields from Clandestine Laboratory Synthesis Routes
Edwin G. Albers, DEA – South Central Laboratory, 1880 Regal Row, Dallas, Texas 75235

Forensic chemists are frequently called upon to estimate production yields in clandestine laboratory cases based upon either the quantities of starting materials present or the size of the empty reaction vessels. Theoretical yields may be calculated; however, these do not reflect the realities occurring in chemical combinations during a synthesis reaction. Because there is a bewildering array of possible conditions and circumstances in a laboratory and none of these are specified when an estimate is called for, assumptions were adopted to impose some order and “typicalness” on the situation. Reactions were run several times and yields factors were calculated.

Illness Reports in Clandestine Drug Laboratory Investigators: A Pilot Study.
Jeffery L. Burgess, MD, Washington Poison Center, P.O. Box 5371, CG-09, Seattle, WA 98115

A retrospective cohort study was done in an international group of 46 law enforcement chemists and in 13 state and local clandestine drug laboratory team members with over 2800 combined responses. Each participant completed a questionnaire concerning previous drug lab responses and adverse health effects during response activities. Methamphetamine labs accounted for 81-97% of all responses. Total illness incident rates varied between 0.75-3.4% of responses. Most exposures were through inhalation, and many occurred in the years prior to use of full personal protective equipment. Symptoms were primarily those of headache and respiratory/mucous membrane irritation. 86% of illnesses occurred during processing, which accounted for 87% of all lab hours. No phase of response activities appeared to carry a higher risk of illness after adjusting for total hours. A majority of illness episodes occurred in labs with leak/spills, fire/explosion, or uncontrolled reactions. Gender and age were not risk factors for becoming ill. Responding to an active lab carried a 7-15 fold risk of becoming ill as compared with set-up, in-transit, or former (equipment removed) labs. The sample size was not large enough to compute risk factors for non-methamphetamine labs or compare the efficacy of different types of personal protective equipment.

The Sodium-Ammonia ‘Nazi’ Method of Methamphetamine Synthesis
Nick Dawson, Arkansas State Crime Lab, #3 Natural Resources Drive, Little Rock, Arkansas 72215

The Missouri and Arkansas region has seen a new clandestine lab method appear in the last two years, which utilizes sodium metal, anhydrous ammonia, and denatured alcohol. Termed the “Nazi” method, because of a World War II patent using these methods, it poses a significant problem for law enforcement and lab personnel alike, as it is a very quick, cheap and efficient method, but one that poses many safety hazards. Originally derived from a metal reduction process for making methamphetamine found in California in the late 1980’s there is a good chance that because of its simplicity and quickness more labs will be seized that have used the “Nazi” method.

Application of the Ionscan for the Detection of Methamphetamine and Ephedrine in Abandoned Clandestine Laboratories
Patricia A. Brown and Jeffrey H. Comparin, DEA – Southwestern Laboratory, 410 W. 35th Street, National City, CA 91950

Clandestine methamphetamine laboratories are prevalent in southern California. The most common encountered synthesis results in vapor release, and drug residue being left behind. The suspected manufacturing area can be vacuumed and/or methanol wiped and screened immediately at the lab site using the Ionscan. Positive results are confirmed by obtaining vacuum sweep samples with subsequent analysis at the DEA laboratory. This procedure has been utilized successfully for identifying methamphetamine and ephedrine from clandestine laboratories that have been abandoned and/or remodeled.

Identification And Quantitation Of Hydriodic Acid Manufactured From Iodine, Red Phosphorus And Water
Scott R. Oulton and Harry F. Skinner, DEA – Southwestern Laboratory, 410 W. 35th Street, National City, CA  91950

Laboratory operators typically have chosen the route of synthesis for hydriodic acid by the reaction of iodine, red phosphorus and water. Other routes of synthesis includes the use of hypophosphorus and phosphorus acids coupled with iodine. Due to these manufacturing processes, phosphoric acid is one of the remaining byproducts. Hydriodic acid prepared commercially is distilled to remove the phosphoric acid. Clandestine hydriodic acid is not typically purified or distilled and therefore an appreciable amount of phosphoric acid is present in the mixture. Commercial and clandestine HI can be differentiated and positively identified. Quantitation of hydriodic acid can be estimated utilizing density or accurately quantitated by an acid/base titration. Acid samples that contain only hydriodic acid are, in all probability, from a commercial source. Acid samples that contain a mixture of hydriodic acid and an appreciable amount of phosphoric acid are of clandestine origin.

Screening Of Illicit Tablets Using The Ionscan
Patricia A. Brown and Pamela R. Smith, DEA – Southwestern Laboratory, 410 W. 35th Street, National City, CA  91950

Recently, the Southwest laboratory has encountered many clandestinely manufactured tablets, both in the field and as evidence submissions. Many of these tablets are similar in appearance, or look like one type of tablet, but contain another substance. These tablets either respond the same to field test kits, or have no response. In the laboratory they may not have a screening test other than chromatography. Therefore, a quick screening method is needed to presumptively identify the tablets. This is done by wiping the tablet onto the clean filter and then screening on the Ionscan. This procedure was used to differentiate 3,4-methylenedioxymethamphetamine and 3,4-methylenedioxyethylamphetamine. The procedure can also be used to differentiate diazepam, methaqualone, and flurazepam.

Outside Testing Laboratories: Friend or Foe?
Jason W. Freed, National Medical Services, 2300 Stratford Ave., Willow Grove, PA 19090

After clandestine drug laboratories are seized, specimens collected, and testing complete, it is inevitable that defense attorney intervention is close behind. Defense attorneys turn to the private sector to miraculously find the solution to the government’s misinterpretation of their clients chemistry curiosity. The role of the private laboratory is one of a check and balance system for the prosecution’s scientific findings. This role should not always be viewed as a hostile attack. Work can vary from educating defense attorneys about a controlled substance or manufacturing procedure to reviewing laboratory testing procedures and results to actual re-analysis of evidence. This presentation will cover some of the approaches taken when working with a seized laboratory already processed by a government crime laboratory. A review of several clandestine laboratories having different levels of involvement will be discussed.

Review of Clandestine Laboratories in Northern New Zealand
Rodney J. Norris, Institute of Environmental Science & Research Ltd. (ESR), Mt. Albert Science Centre, Hampstead Road, Mt. Albert Private Bag 92-021, Auckland, New Zealand

Several types of interesting clandestine drug laboratories have been encountered in the northern part of New Zealand in recent years (as well as the regular occurrence of hash oil and homebake laboratories). My laboratory’s involvement will be discussed, and as much information as possible regarding each type of lab will be reviewed.

Unusual and interesting laboratories have included:

MDMA (Ecstasy) being manufactured at a will-known alternative community.

Alkyl nitrites being supplied for the “adult” market.

PCP manufacture.

In the absence of an operating methamphetamine laboratory being found in our region, attempts to manufacture methamphetamine will be discussed. Some interesting literature seized by the police and customs will be illustrated.

Bombs And Booby Traps In Clandestine Labs
S/A Alexander F. Smith, Jr., Drug Enforcement Administration, Baltimore, MD

This workshop will present the recognition and awareness of explosive materials; the component parts required for the construction, placement, activation, and blast effects of improvised explosive devices; current counter-measure equipment and strategies directed by drug trafficking individuals and organizations to repel law enforcement operations. Reference materials are provided and the presentation is complemented by extensive slide and video aids.

Cocaine Processing
John Casale, Senior Forensic Chemist, Drug Enforcement Administration, Special Testing and Research Laboratory, 7704 Old Springhouse Road, McLean, VA  22102-3494

The predominant methods currently utilized in South America for illicit production of cocaine are described. These include the production of cocaine base from cocaine paste from coca leaf via both the solvent and acid extraction techniques, and conversion of cocaine base to cocaine hydrochloride.

Clandestine Production Of Amphetamine And Its Analogs: The UK Perspective
Leslie A. King, Ph.D., Forensic Science Service, Aldermaston, Berkshire, U.K.  RG7 4PN

Seizures of amphetamine and various of its derivatives are increasing at a faster rate than other illicit drugs. Impurity profiling has enabled the major sources of amphetamine to be identified. Introduction of increasingly strict precursor controls has forced most production overseas, but around fifteen clandestine laboratories are found each year. One of the largest laboratories was raided in 1993; several tons of unused precursors were recovered. At another site earlier this year, operators were using a 500L steel vessel for production of phenyl-2-propanone. In the past few years, many new amphetamine analogs have appeared; most are not controlled by legislation and some present analytical challenges.

Clandestine Laboratories And Chemical Seizures In The United States and Worldwide
Debbie Wegman, Drug Enforcement Administration, Office of Diversion Control, Drug and Chemical Evaluation Section, 600 Army-Navy Drive, Washington D.C.  20532-0001

The United States is a party to the United Nations Convention against Illicit Traffic in Narcotic Drugs and Psychotropic Substances, 1988 (1988 Convention).   As a party to the 1988 Convention, the United States must submit specific chemical information to the United Nations on an annual basis: quantities seized, seizures by country of origin, methods of diversion and illicit manufacture, licit and illicit use, and importation/exportation. The United States submissions as well as other countries submissions will be discussed.

Kodak Film Developing Chemicals And Clandestine Methamphetamine Laboratories: An Apparent Motive for Homicide
Katherine S. Wilcox, Oregon State Police Forensic Laboratory, 333 4th Avenue, Coos Bay, OR  97420

On two previous field investigations of clandestine methamphetamine laboratories, bottles of Kodak developing solution have been found among the chemicals. In this case presentation, two boxes of miscellaneous photographic chemicals were the apparent motive for two “cranksters” to murder their associate. The murderers thought the photographic chemicals (which were worthless junk) to be worth $250,000 to $300,000 if they could just find a cook to extract the precursor chemicals. When they thought their associate was holding out on them, he was murdered, and burned up in his new car. The myth that essential precursors can be extracted from photographic chemicals will be explored.

Discovery Of A Clandestine Laboratory In Transit In The Port Of Antwerpen, Belgium
V.Arescchka, C. van Haeren, H, Coppens, B. Viaene, and V. Eckelmans; National Instituut voor Criminalistiek en Criminologie, Brussels, Belgium

Twelve suspicious metal containers (each approx. 33 m3) were found in the port of Antwerpen, Belgium. When opened, they appeared to contain all the necessary equipment for a large scale clandestine laboratory. The confiscated equipment indicated a high degree of sophistication by its operators.

Among the items seized were the following:

an electrical generator (400Kw capacity)

water recycling equipment

two high speed tablet presses (Unipress) with a capacity of 100,000 tablets/hour

twenty boxes of tablet molds (one with a dove symbol)

heat exchangers

water cooling systems

reactor for drug synthesis with several cubic meter capacity

No large supply of chemicals was ever found. Only one tablet with the dove logo was found. Chemical analysis with the aid of Gas Chromatography coupled to Mass Spectrometry (GC/MS) techniques revealed the presence of 3,4-methylenedioxy-N-methamphetamine (MDMA or XTC). This compound was also identified in the powder discovered in and around the tablet presses and on some of the apparatus. Traces of precursor material (e.g. isosafrole) and of chemical intermediates (e.g., N-formyl-MDMA) typical for the Leuckart synthesis were also detected.

Cultivation Of Cannabis Seeds Seized From A Retail Store Called HEMP BC: Examination of THC Purity and Chemical Profiles
Richard R. Laing, Health Canada, Health Protection Branch, 3155 Willingdon Green, Burnaby, BC V5G4P2

In Vancouver, BC there is a strong movement to decriminalize Hemp (Cannabis sativa). Most activists claim that hemp should have a legitimate place in society and the Hemp BC retail store sells everything from hemp clothing, hemp flour, foodstuffs, and cannabis seed. In January, 1996, Vancouver City Police raided the storefront and seized numerous quantities of cannabis seeds. Most of these seeds were packaged in small numbers and had names such as Primo Cut, Mighty Mite, and Thick Gulf Indica Prices ranged from $1.50 to $4.00 a seed. Under the Narcotic Control Act, non-viable cannabis seeds is permitted in bird food while viable seed is illegal. Various types of cannabis seeds were grown under identical conditions in order to determine if the cot per seed reflected the THC concentration. This poster presents this data along with sample matching data of similar seeds and examines chemical profiling based upon sex and effects of female plants going to seed.

Coca Leaf Alkaloids And Illicit Cocaine Signature
James M. Moore and John F. Casale, DEA Special Testing and Research Laboratory, 7704 Old Springhouse Road, McLean, VA  22102-3494

Methodology for the isolation and identification of coca leaf alkaloids is described. Their relationship to the development of illicit cocaine signature methods.

Speed Changes: August 1995. A Lower Gear?
Jerry Massetti, California State Department of Justice, Fresno Regional Laboratory, 6014 North Cedar Avenue, Fresno, CA 93710

On August 19, 1995, d,l-amphetamine began showing up in suspected methamphetamine samples submitted to CA DOJ crime laboratories. Amphetamine had been a rarity since the mid-1980’s. Despite this, within a few weeks of its first appearance, d,l-amphetamine and d-methamphetamine mixtures were detected in suspected methamphetamine samples by crime laboratories in at least six Western US states. Midwest and Eastern US labs reported it by late November.
At the same time as amphetamine appeared, the amount of active phenethylamine ingredient dropped dramatically. Very large amounts of caffeine and nicotinamide were used as diluents. An increasing number of samples were also found to be diluted with dimethylsulfone. Changes in the physical appearance of samples corresponding to chemical changes were also noticed.
d,l-Phenylpropanolamine has been substituted for single isomer ephedrine or pseudoephedrine in large scale clandestine laboratories using the hydriodic acid and red phosphorus reduction. Phenylpropanolamine is being extracted from commercially available tablets such as AcceleRx Appetite Suppressant (M.A. Products, Pinellas Park, FL). Secondary medicinal compounds like triprolidine and chlorpheniramine carry over into the final clandestinely manufactured products.
d,l-Amphetamine continues to persist in suspected methamphetamine samples one full year after it first emerged. Amphetamine was present in 14% of approximately 3,000 California State Department of Justice (CA DOJ) drug cases in which either amphetamine or methamphetamine were identified during the first six months of 1996. This figure varied from 8% to 30% amphetamine in suspected methamphetamine samples when data was considered individually from each of the 10 CA DOJ laboratories that perform dosage drug analyses.

«Trace Drug Evidence Collection Techniques»
William M. Moriwaki, DEA Western Lab, San Francisco, California, USA

Ever since the O.J. Simpson trial unfolded, trace evidence collection and preservation has been closely scrutinized by the courts. The possible contamination and integrity of the evidence are the usual concerns.  However, collecting trace drug evidence can present additional challenges. At the Drug Enforcement Administration’s Western Laboratory in San Francisco, we have successfully used two different procedures to collect trace amounts of drugs. One is based on the classic vacuum sweeping technique and the other is a solvent swabbing technique.
The vacuum sweep is a classic technique used to collect trace physical evidence such as hairs, fibers, and drugs. Unfortunately, cross contamination is possible when collecting trace evidence with a vacuum. The nozzle head and filter housing must be thoroughly cleaned between each collection. Using clean pre-packaged disposable vacuum filter nozzles solves the issue of sample contamination. These filters also increase efficiency because «blanks» no longer need to be collected between different samples.
An alcohol wipe is the second technique we successfully use to collect drug residues at crime scenes and from drug suspects. Carrying methanol for swabbing can be problematic:  bottles can break or leak. Federal law restricts carrying quantities of flammable liquids on airline flights. Contamination of the alcohol may be an issue, thus requiring «blanks» to be taken before each swabbing. A solution to the logistic problems of this technique is to use commercially prepared, pre-packaged, and pre-moistened alcohol towelettes. These towelettes offer a clean, compact, and contamination-free way to collect drug residues. These towelettes are an inexpensive and viable alternative to carrying solvents to a crime scene.
To help identify areas where trace amounts of drugs may be present, an instrument known as the Ion Scan has been successfully used. The advantages and disadvantages will be discussed.

«Clandestine Phenethylamine Laboratory Syntheses and Analytical Training»
Roger A. Ely, DEA Western Laboratory, San Francisco, CA, USA

Regardless of their experience in examining suspected controlled substances, newly hired forensic chemists with the U.S. Drug Enforcement Administration’s (DEA) laboratories must successfully complete a rigorous analytical training program before they are allowed to examine case samples. Since the types of cases and work load vary with each DEA laboratory, each laboratory’s training program is developed and tailored to suit their needs.
The DEA Western Laboratory, San Francisco, training introduces the controlled and restricted drug groups including color screening tests, extractions, identification and quantitative analyses procedures, and mock court sessions. The program also familiarizes the trainee with the uses and limitations of analytical instrumentation in the Western Laboratory. Though one or two «senior» chemists lead the training, other staff chemists assist by providing specialized training in analytical and/or instrumental methodology for particular drugs.
Over the past 5 years, the author has developed and refined the clandestine phenethylamine laboratory investigation and analyses portion of the Western Laboratory’s training program. This section gives the new chemist the basic knowledge, skills, and techniques necessary to investigate, analyze, and testify about clandestine phenethylamine laboratories seized in the Western Laboratory’s 11-state service area. The training utilizes classroom lecture, hands-on syntheses and sampling, hands-on analytical methodology, a written examination and an oral presentation of analytical findings.
This presentation details the clandestine phenethylamine training designed by the author. The author will provide a critical assessment of the success of the training to date and offer suggestions for developing similar training programs for individual laboratories.

«Separation and Identification of Ephedrine and Pseudoephedrine Mixtures»
Scott Oulton, DEA Southwestern Laboratory, National City, CA. USA

Clandestine methamphetamine laboratories are prevalent in the United States, especially in southern California. The synthesis route of choice is the reduction of ephedrine or pseudoephedrine with hydriodic acid and red phosphorus. Due to their availability, combinations of these two precursors are common at laboratory sites. Since ephedrine and pseudoephedrine are diastereoisomers, the chromatographic and physical separations of these two isomers are difficult.
Trace mixtures of ephedrine and pseudoephedrine can be extremely difficult to analyze utilizing common underivatized chromatographic techniques. Separation and detection of ephedrine and pseudoephedrine mixtures can be accomplished with a gas chromatograph equipped with an HP-50+ (cross-linked 50% phenyl methyl siloxane) column. This mid-polarity phase column effectively separates ephedrine and pseudoephedrine mixtures without having to utilize derivatization techniques. Identification can be performed utilizing a gas chromatograph equipped with an HP-50+ column and an infrared detector.
With sufficient sample size, separation and isolation of ephedrine and pseudoephedrine can be accomplished by simple dry extraction techniques. Identification of these compound mixtures can be performed utilizing infrared spectrophotometry.

«Possible False Identification of MDEA and Tracing Back Synthetic Pathways in a Clandestine Laboratory»
C. van Haeren, V. Areschka and H, Coppens, National Institute of Forensic Science, Brussels, Belgium

Twelve suspicious, metal containers were discovered in the Port of Antwerpen, Belgium. They contained all the necessary equipment for a clandestine laboratory.
From the GC-MS analysis of the material, found in and around the equipment, it was clear that XTC was produced. Interpretation of the chromatograms and the mass spectrum data revealed that the main peak corresponded to 3,4-methylenedioxy-N-methylamphetamine (MDMA). A smaller peak was identified as 3,4-methylenedioxyamphetamine. A second small peak appeared to be 3,4-methylenedioxy-N-ethylamphetamine (MDEA).
Further examination of the findings, however, suggests that the second small peak corresponds to N,N-dimethyl-MDA instead of MDEA. This fact could not be proven directly because commercial standards for N,N-dimethyl-MDA and MDEA are not available.
The following indirect arguments were considered:

The unidentified peak is symmetrical, whereas the peak corresponding to MDEA gives a slightly more tailing profile due to the NH group in this molecule.

The mass spectrum of the unknown substance and MDEA are identical, except for the signal at m/z= 96, which is smaller in the case of MDEA.

TFAA derivatization of the found material yields MDMA-TFA and MDA-TFA, while no MDEA-TFA can be detected. This appears to confirm the absence of a NH group in the compound.

When MDEA, extracted from known MDEA tablets, was added to the found material; the resultant chromatogram showed that MDEA eluted at a different time than the unidentified peak.

These arguments make it highly probable that N,N-dimethyl-MDA was present in the found material. This conclusion is important, because the correct identification of the by-products of the synthesis of MDMA can help to elucidate the pathways followed in the clandestine production. The presence of N,N-dimethyl-MDA and MDA in trace amounts indicates that the MDMA was produced by the methylation of MDA and not from the hydrolization of N-formyl-MDMA.

«Fester Revisited: Comments On Proposed MDMA Synthesis»
Vincent Murtagh, Australian Government Analytical Labs, Pymble, NSW, Australia

In the second and third editions of his book, «Secrets of Methamphetamine Manufacture,» Uncle Fester proposed the Ritter reaction for making MDA. This process has been analyzed by various groups and the general view suggests that is not successful for ring-substituted amphetamines. In his fourth edition, Fester agrees. He now suggests the halo-safrole route.
In this presentation some remarks are offered regarding the feasibility of use of the new method for clandestine cooks, based on some Sydney, Australia seizures.

«Three Fatalities Involving Phosphine Gas, Produced as a Result of Methamphetamine Manufacturing»
Lynn J. Willers-Russo, Los Angeles County Sheriff’s Department, Scientific Services Bureau, Los Angeles, CA, USA

This paper presents a case involving the death of three individuals suspected to have been overcome by phosphine gas. Phosphine is a toxic gas which can be generated during the manufacturing of methamphetamine. The objectives of this paper are to discuss:

The chemical mechanisms behind the generation of phosphine gas as they relate to the manufacturing of methamphetamine;

The toxicity of phosphine gas and the symptomology due to inhalation;

Possible phosphine exposure in the field by criminalists and law enforcement personnel who respond to clandestine laboratories.

In August of 1996, three deceased individuals were discovered in a small motel room in Los Angeles County. Responding deputies who assessed the scene noted chemicals and glassware consistent with the clandestine manufacture of methamphetamine. A possible by-product of the ephedrine / hydriodic acid / red phosphorus manufacturing method is phosphine gas. This gas is extremely poisonous and can be generated when the reaction mixture is overheated. As no visible signs of injury were apparent on the victims, phosphine poisoning was suspected by responding Clandestine Laboratory Task Force personnel. Drager tubes were used to test for the presence of phosphine gas, which was detected at levels in excess of 1.0 ppm. The Threshold Limit Value is 0.3 ppm. There was concern regarding the exposure of deputies who had initially assessed the scene with no protective equipment to this potentially lethal gas.
Clandestine laboratories are routinely encountered in Los Angeles County and frequently involve crude conditions and poor ventilation. The August 1996 incident raised several concerns and questions regarding lethal exposure, symptomology, general toxicity and the chemistry of phosphine gas. Initial review of the standard available reference material revealed little information. In an attempt to adequately address these new concerns, a more extensive review of scientific literature was conducted, and persons with specific knowledge or experience with phosphine gas, were contacted.
Phosphine (hydrogen phosphide) is a toxic, colorless gas, which can be produced by a variety of chemical reactions. Generally, phosphine is seen in the farming industry where it is used as a grain fumigant. It has long been known that phosphine can also be generated during the manufacturing of methamphetamine, using ephedrine, hydriodic acid and red phosphorus. Although some information about phosphine chemistry is available, there are no direct references to the generation of phosphine as a by-product, during the manufacturing of methamphetamine. Some references however, were noted involving a reaction with phosphorus acid, whose chemical mechanism seems likely, given the type of clandestine labs that we frequently encounter.
Most of the scientific literature regarding phosphine exposure deals with the inhalation of the gas by grain fumigators. The symptomology is well documented. The more common symptoms include those involving the lungs and respiratory tract. Bronchitis and irritation of the lungs, dyspnea and pulmonary edema are frequently seen. Other common symptoms include headache, fatigue, dizziness, pain or pressure in the chest, nausea and vomiting. The primary result at autopsy is generally pulmonary edema, and this case was no exception. Some studies indicate a correlation between phosphine exposure and the inhibition of electron transport, due to the phosphine interaction with cytochrome oxidase. Research has also associated phosphine with possible chromosomal damage and with Heinz body formation in red blood cells.
With respect to possible phosphine exposure from clandestine laboratories it is unknown to what extent, if any, responding personnel are exposed, as no testing for the gas is routinely performed. As a result of this deadly incident, a Drager pump and tubes for phosphine (as well as a phosphine-specific gas mask) were purchased and utilized in the field, when the presence of phosphine might be likely. The results were surprising in that phosphine was encountered more often than originally suspected. Once the odor was recognized, the number of incidents where it was detected increased, more likely due to the increased awareness than by an increase in the actual number of occurrences. Some of the criminalists noted that they had previously encountered the odor before, both in the field and in laboratory submissions. The review of this material has led to a better understanding of phosphine, and has allowed us to educate our criminalists and other field personnel, to the possible hazards of accidental exposure.

«Imitation Liquids for Clandestine Laboratory Investigations»
Norman E. Mausolf, DEA – Mid-Atlantic Lab, Washington D.C., USA

Recipes for liquids that can imitate «liquid» PCP, phenylmagnesium bromide solution, and piperidine are given. The chemicals used are not controlled and are less hazardous than their genuine counterparts. An attempt has been made to imitate appearance as well as smell.

«A Statistical and Geographic Study of Methamphetamine and Amphetamine Submissions to the Mississippi Crime Laboratory from January 1996 through June 1997»
Jamela Naron Johnson, Mississippi Crime Laboratory, Meridian, MS, USA

This study was performed to provide a «first-hand» analyst account of methamphetamine and/or amphetamine submissions to the Mississippi Crime Laboratory from January 1996 through June 1997 for the purpose of illustrating the recent stimulant trends in the State of Mississippi. The primary objectives of this study are:

To illustrate specific county distribution, noting any social considerations which could reveal a link between stimulant abuse and each particular county (i.e. high incidence of motorcycle gangs, college towns, truck drivers, military installations, etc.);

Diluent trends in specific areas of the State of Mississippi; and

Concurrent case exhibits containing other controlled as well as non-controlled substances.

«l-Methamphetamine in the Midwest»
Gerald T. Skowronski, DEA – North Central Laboratory, Chicago, IL, USA

Seven exhibits containing l-methamphetamine were analyzed by the DEA – North Central Laboratory early in 1997. Analytical data including polarimetry and derivatized gas chromatography used for the enantiomer determination is presented.

«Bunk Mini Thins»
Gina Williams, San Bernardino County Sheriff’s Dept., Scientific Investigations Division, San Bernardino, CA, USA

San Bernardino County Sheriff’s seized 100 cases of Mini–Thin tablets bearing two different lot numbers. All bottles were factory labeled and factory sealed. Pills from one lot number contained pseudoephedrine as expected. Pills from the other lot number contained no pseudoephedrine and were not visually similar.  Both types of pills and analytical data are displayed.

«Hydrogen Sulfide Fatality»
Mahul Anjaria, Blaine Kern and Kerri Heward; San Bernardino County Sheriff’s Department, Scientific Investigation Division, San Bernardino, CA, USA

A deceased male found lying outside of a room which contained a methamphetamine laboratory. Inside of the room was found a discharging gas cylinder labeled «hydrogen sulfide» which was connected to tubing leading into a bucket of liquid. An APR with organic vapor cartridges was found near the body. Apparently, the «cook» mistakenly used hydrogen sulfide gas instead of hydrogen chloride gas to salt out his finished product, leading to his demise.

«Determinations of Cations in Seized Clandestine Laboratory Samples by Capillary Electrophoresis»
Victor A. Bravenec, DEA South Central Laboratory, Dallas, TX, USA

Many synthesis routes use inorganic components to manufacture illicit drugs. The analysis of these inorganic components in clandestine laboratory samples can prove to be valuable information in determining the synthesis route used. Capillary Ion Electrophoresis (CIE) was chosen for the analysis of the cations as it provides good selectivity, short analysis time, smaller amount of sample (4-7hl), little sample preparation, and equal or lower detection limits (5 to 30 ppb) when compared to ion chromatography or atomic absorption spectrometry. Capillary Ion Electrophoresis is a capillary electrophoresis technique optimized for the rapid determination of low molecular weight inorganic and organic ions. These small ions lack a chromophore so Indirect Photometric Detection (IPD) is employed to obtain detection of these analytes. The following cations are characterized: aluminum, chromium, sodium, lithium, magnesium, ammonium, barium, zinc, lead, calcium, copper, nickel, strontium, potassium, mercury, and thorium. Analysis of illicit samples of popular synthetic routes will be presented as well as detection of various cations on clandestine glassware and other containers.

«Dirt Extraction of Methamphetamine»
Kerri T. Heward and Ken Lee; San Bernardino County Sheriff’s Department, Scientific Investigations Division, San Bernardino, CA, USA

In the past two years the San Bernardino County Sheriff’s Department – Scientific Investigations Division has seen numerous methamphetamine laboratories involving a «dirt extraction» procedure. These laboratories have all been associated with a Mexican National style dump site in the Lucerne Valley which was not adequately remediated.
Observations and analysis of samples taken by the crime lab show that methamphetamine can, in fact, be extracted from the dirt on the property in question in significant amounts.

«Anion Analysis of Hydriodic Acid by Capillary Electrophoresis»
Nathan Salazar, DEA Southwestern Laboratory, San Diego, CA, USA

Anion analysis of hydriodic acid (HI) was conducted using capillary electrophoresis (CE) with indirect photometric detection. Analysis were carried out using a fused silica 70cm (61.5cm effective length) x 75m I.D. capillary at 25°C, with 30kV applied potential. The background electrolyte consisted of 2.25mM pyromelletic acid as the visualizing agent, and 0.75mM hexamethonium hydroxide as an electroosmotic flow modifier. The background electrolyte was buffered at pH 7.7 with sodium hydroxide and triethanolamine. Separation of iodide from other anions was achieved by addition of 10% methanol to the background electrolyte. Quantitation of iodide was conducted to determine the percent HI in solution with an observed linear dynamic range from 15 to 120 ppm. Clandestinely prepared HI made by reacting iodine with phosphorus in water was compared to commercially prepared HI. Detection of phosphate anion was observed for the clandestinely prepared HI, whereas commercially prepared HI displayed no detection of phosphate anion.

WORKSHOPS

Carbonyl and Amine Chemistry: Continued
Harry F. Skinner, DEA Southwest Laboratory, San Diego, CA, USA

Continuing last years presentation examples will be given to define an analytical scheme based on the pH of solutions found at clandestine laboratory sites,

Ion Mobility Spectrometry Demonstration
Bryan A, Henderson, DEA Southwest Laboratory, San Diego, CA, USA

Ion Mobility Spectrometry is a valuable tool in the detection of trace amounts of drugs. An overview of the theory will be offered. This will include a practical demonstration of this technique in a simulation of field sampling modes.

Clandestine Laboratory Sample Characterization and Extraction Techniques
Roger A. Ely, DEA Western Laboratory, San Francisco, CA, USA

One of the challenges for the forensic chemist is characterizing seized clandestine laboratory samples and applying a suitable extraction scheme for isolating controlled substances, precursors, reagents, and/or solvents. In this workshop, the author has classified various types of clandestine lab samples and created a flow chart to guide the examining chemist in selecting a suitable extraction method. This workshop will cover the examination of one- and two-phase liquids miscible and immiscible with water, liquid samples containing solids, solid organics and inorganics, residues, and specialized samples such as vacuum pump oils. This workshop will discuss each of the presented extraction methodologies, and provide tips on performing the extractions. Other topics to be discussed include the quantitative analysis of methamphetamine and amphetamine by GC-FID, the identification of the optical isomers of the phenylisopropylamines by derivatization using GC-FID, and some tips for improving phenethylamine chromatography.

Court Room Presentations
Roger A. Ely, DEA Western Laboratory, San Francisco, CA, USA

The ultimate test of the forensic drug chemists expertise is in the arena of the court. Testimony regarding clandestine laboratory evidence, processes, and reconstructions are very different from the typical controlled substance identification testimony. The success or failure of a forensic chemist’s testimony regarding a clandestine laboratory is directly related to the witness’s training, preparation, experience and breadth of knowledge. The presentation of often seemingly complex and technical concepts in a manner that a jury or court can understand is a challenge; yet, adequate preparation and rehearsal allow the witness to easily convey complicated information in a simple manner. The use of court displays cannot be understated. This workshop will provide some suggestions and salient points to consider for the clandestine laboratory expert witness.

Frye vs. Daubert: How Much Meth Could A One-Armed Man Cook, If A One-Armed Man Could Cook
Pamela Johnson, Semo Regional Crime Lab, Cape Girardeau, MO, USA

The raid on a clandestine laboratory in Park Hills, Missouri, resulted in the recovery of a number of full and empty pseudoephedrine tablet boxes and bottles. These were inventoried, photographed, and released to the hazardous material disposal unit.
The DEA agents and the local police department put questions to the laboratory as to how much methamphetamine could have been produced. Calculations were conducted on how much pseudoephedrine was present and how much methamphetamine could have been produced if the reaction resulted in 100% conversion. Since the sodium/ammonia reduction reaction was reported at the time to result in 90% conversion, a yield projection at this level was provided. The prosecution decided to utilize these projections in their court case. The use of these calculations were challenged and a Frye vs. Daubert hearing was conducted prior to the criminal trial.

Production Capacity Reports
Gerald Skrowonski, DEA North Central Laboratory, Chicago, IL, USA

A forensic chemist may not only have to analyze evidentiary samples from a clandestine laboratory, but may also be called upon by prosecutors to prepare a Production Capacity Report. The purpose of this presentation is to present several ideas on how to prepare these reports.
The total amount of controlled substance is typically calculated from the samples analyzed in the case. In addition, forensic chemists are required to determine how much more could be made from chemical supplies present at the clandestine laboratory. Historically, the production capability has always been calculated as the amount of controlled substance that could be manufactured at the 100% theoretical yield. This approach has been affirmed by two court decisions (1,2).
The data that the forensic, chemist needs to perform these calculations may be based on:
I. Primary Precursors
A) Tablets
1. Listed Strength
2. Actual analysis
B) Liquids
1. Instrumental techniques (GC, LC, etc.)
2. Gravimetric
C) Powders
1. Net weight
2. Actual analysis
3. Residue on filter paper
II. Important Reagents

When one has a recipe or notes listing the amount of the reagent used for a particular size synthesis batch, the values listed may be used.  Occasionally, records (handwritten notes, computer data, etc.) are found at clandestine lab sites indicating past drug production. The total amount of drug made can be evaluated from this information and, if pertinent, be included in the report.
Finally, while a reasonable percent yield for the particular synthesis employed in the clandestine laboratory is not included in the capacity report, the forensic chemist should be prepared to testify to such a value and have the literature reference and/or other evidence available to support this value

United State v. Wagner, 884 F.2d 1090 (8th Cir. 1989) (Maximum amount of methamphetamine that defendant could produce was used in determining base offense level even though defendant inexperienced).

United States v. Beshore, 96 F.2d 1380, 1383 (8th Cir, 1992) (The defendant’s purpose here was to manufacture methamphetamine, therefore any calculation must be based on the total amount of methamphetamine that the defendant was in a position to produce).

Mexican Drug Trafficking Situation Brief
Robert N. Evans and Thomas J. Harding, DEA EPIC Operational Intelligence Unit, El Paso, TX, USA

An overview of drug-trafficking organizations operating in Mexico and the United States. Personalities will be identified, along with a historical perspective of the Mexican Drug Trafficking Organization. Current methodology being utilized by these organizations will be detailed, as well as the relationship to criminal organizations operating along the U.S./Mexico border.

A Cookers Dream
Eric L. Lawrence, Indiana State Police, Indianapolis, IN, USA

On February 13, 1997 search warrants were served at two locations southwest of Indianapolis. Eight individuals, part of a distribution ring dealing in methamphetamine, were arrested. One of the individuals arrested was charged with the manufacture of methamphetamine. What makes this case unusual is not only that the “cook” was employed by a large pharmaceutical company; but, was novel in his approach to the manufacture of methamphetamine. The location of his lab and the synthesis routes used were unusual. Both of these issues will be discussed. At the end of this presentation — a taped interview with the “cook” explaining how he made the dope will be viewed.

Tryptamines and TIHKAL
Andrew C. Allen, Ph.D., SmithKline Beecham Pharmaceuticals, King of Prussia, PA, USA

Tryptamines and their significance to forensic science are the subject of this presentation. The topics of discussion will include:

The synthesis of DMT and related analogs;

The synthesis of indole and substituted indoles;

Commercial sources of indole analogs as precursors to tryptamine analogs;

The pharmacology of tryptamine derivatives in terms of structure activity relationships;

Shamanism and its historic role in the use of these hallucinogenics; and finally,

Animal and botanical sources of tryptamines and related analogs.

Protecting Group Chemistry
Tim McKibben, Aurora Police Department, Aurora, CO, USA

Protecting group chemistry involves the use of reagents to convert a functional group into a protected functional group, which can then be subjected to reaction conditions, which would otherwise destroy the unprotected form. This technique is commonly used throughout organic chemistry, especially in the pharmaceutical industry. This presentation will introduce the forensic chemist to some common protection groups and techniques used to add and remove them from the chemical intermediate. These “protected“ intermediates or precursors have been encountered by forensic chemists and should be familiar to chemists investigating illicit drug manufacturing cases. Examples of protection group chemistry used in illicit and legal manufacturing will be presented.

The Kathey James Story
D.D.A. John M. Davis, Riverside County District Attorney, Riverside, CA, USA

The Kathey James story and the new cases currently in the system will be used to illustrate the prosecution of homicides arising out of clandestine laboratory incidents. The future of case law in this area will be discussed and the successes and failures in the legislative arena. It will also be shown why child endangerment is not a viable theory for criminal liability in a murder trial.

A Career High
Richard R. Laing, Health Canada, Burnaby, BC, Canada

Question: What do you have when you seize large quantities of LSD, MDA, MDMA, and DMT in a clandestine lab setting?

Answer:  Conspiracy, sophisticated laboratory setup, international distribution networks, multiple identities, and multimillion-dollar production capacity.

All of these were found in a Vancouver suburban clandestine laboratory that was seized September 26, 1996, following a lengthy investigation. To add intrigue to this case, enter the key figure of Nicholas Sand. He had been a fugitive for over 20 years; convicted in absentia for the manufacture of LSD. The seized chemicals, notes, and ledger sheets all depict a large commercial manufacture and distribution operation. In the year proceeding the seizure, the records indicated gross wholesale sales in excess of $1,866,000.00. These sales represented the distribution of 127 gm of LSD, 500 gm of MDA, 4800 gm of MDMA, and 235 gm of DMT.

Cook” Fails Chem 101; Hydrogen Sulfide Fatality

Mehul B. Anjaria, Criminalist and Hiram K. Evans, Supervising Criminalist / Deputy Sheriff San Bernardino County Sheriff’s Department Scientific Investigations Division 200 S Lena Rd San Bernardino, CA 92408-1604

Abstract

A methamphetamine “cook” equipped with an APR apparently mistakenly attempted to salt out his finished product with hydrogen sulfide rather than hydrogen chloride, leading to his demise.

Text

On January 30, 1997, Criminalists Mehul B. Anjaria and Blaine M. Kern responded to a suspected clandestine drug laboratory in the Muscoy area of San Bernardino, CA. On arrival, they were directed by Sheriff’s Narcotics Detectives to the body of a deceased Hispanic male in his late twenties, lying supine on the driveway adjacent to what had been the garage, located to the rear of the residence. Near the body of the deceased was a half-face air purifying respirator (APR) equipped with organic vapor cartridges. The garage, converted to living quarters, had been previously entered by a Sheriff’s Sergeant wearing self-contained breathing apparatus (SCBA) only long enough to ascertain that no other victims/suspects were present and to note a gas cylinder, the open valve on which he was unable to close.

Criminalists Anjaria and Kern donned protective clothing and SCBAs and entered the converted garage, noting a gas cylinder labeled “hydrogen sulfide” with ice formed on the bottom potion of the cylinder, indicating that the cylinder was freely discharging. The cylinder was connected via tubing to a 5 gallon bucket containing liquid, consistent with the final step of methamphetamine manufacture in which the drug is salted out using hydrogen chloride gas. Also present in the building were two-phase liquids, red phosphorus, hydriodic acid, lye, a mop bucket equipped with a press, and other items commonly associated with the clandestine manufacture of methamphetamine. Due to the hazardous nature of the environment, additional air cylinder for the SCBAs were requested.

After conferral between the various law enforcement, fire department and Coroner’s representatives, it was decided to move the body of the deceased upwind from his original position to facilitate the examination of the body.

Criminalists Anjaria and Kern processed the interior of the garage. Supervising Criminalist Hiram Evans and Forensic Specialist Karen Rice assisted the Deputy Coroner with an examination of the body of the deceased, including rolling set of inked fingerprints and recovery of his wallet. The wallet contained some peso notes and a California Driver’s License (CDL), although the CDL photograph did not particularly resemble the victim. Forensic Specialist Rice also assisted in photographing the exterior of the scene.

The inked fingerprints of the deceased were submitted to the Lab’s Cal-ID unit and subsequently identified as those of a Mexican National, but not the name given on the CDL.

Hydrogen sulfide (H2S) is a colorless, heavier than air, flammable gas having the characteristic, pungent odor of rotten eggs. Vapor concentrations as low as 50 ppm in air cause toxic symptoms, 300 ppm is immediately dangerous to life and health (IDLH), and 1000-2000 ppm is usually fatal within minutes [1]. By the way of comparison, hydrogen cyanide (HCN) is also a colorless, flammable gas, having a characteristic faint odor, but in contrast is lighter than air, with a 50 ppm IDLH level. Fatal H2S poisoning may occur even more rapidly than following an exposure to similar concentrations of HCN as hydrogen sulfide does not combine with hemoglobin, but kills through respiratory paralysis [2].

Acid gas, organic vapor, and base cartridges generally utilized in APRs are marked to be used with hydrogen sulfide for escape only. While the odor of hydrogen sulfide is detectable at very low concentrations, it is an insidious irritant and chemical asphyxiant which fatigues the sense of smell. With the sense of smell fatigued, those exposed fail to get warning of high concentrations, leading to respiratory paralysis and sudden collapse [3].

Hydrogen sulfide has been used by Mexican National methamphetamine “cooks” for the clandestine manufacture of hydriodic acid and its is likely the deceased obtained it mistakenly for hydrogen chloride gas. Whether the “cook” obtained it on his own or through others is unknown at this time.

References

1. 1. Clinical Toxicology of Commerical Products, Marion N. Gleason, Robert E. Gosselin, and Harold N. Page, Willaims & Wilkins Co., Baltimore, MD, 1957, p. 147.
   2. Dangerous Properties of Industrial Materials, N. Irving Sax, 2nd ed., Reinhold Pub. Co., New York, NY, 1963, p. 888.

Merck Index, Susan Budavari, ed., 12th ed., Rahway, NJ, 1996, p. 823.

Hypophosphorous Acid Use Increases at California
Clandestine Methamphetamine Labs

Jerry Massetti, Criminalist CA DOJ Crime Lab 1704 E. Bullard Fresno, CA  93710-5856

With increasing frequency, California crime lab personnel who process clandestine lab scenes are recognizing hypophosphorous acid, H3O2P, as a reaction ingredient at clandestine methamphetamine laboratory scenes. In August 1996, a Kern County criminalist reported H3O2P was being used to reduce ephedrine at a clandestine methamphetamine laboratory scene in that county [1]. Since then it has become apparent that H3O2P is being used in most parts of California.

The great majority of H3O2P usage has been almost exclusively at «tweeker» league meth labs where gram-to-ounce size quantities of product are made at a time. Small disposable glassware, such as a canning jar or a beer bottle, is employed to contain the ingredients. No red phosphorous is used. The acid is simply poured onto the starting material and iodine crystals. Reportedly, as little as fifteen minutes of heat has been applied. Efficiency of the reaction procedure is unclear and has not been established from field observations.

One chemist reported that a 12 liter round bottom flask contained a reaction mixture which utilized H3O2P. This large scale reaction using H3O2P is unusual. H3O2P has not been reported to be used as a reactant at large scale (multiple 22 L reaction vessel) methamphetamine laboratories whose investigations commonly associate operatives from Mexico. It has been observed to be used as a stabilizer for hydriodic acid that is clandestinely produced on a large scale by Mexican National operations. In those particular instances approximately 25 ml was added to 5 gallons of hydriodic acid (~52-57%, w/w).

Chemical cash sales reported to the California Bureau of Narcotics Enforcement / Clandestine Lab Enforcement Program (BNE / CLEP) corroborate lab scene observations. Cash sales of chemicals in California exceeding one hundred dollars are required to be reported to BNE/CLEP. In about a two year period ending December 1996, the amount of H3O2P reported to this program has more than tripled from $18,844 to $60,383. One half liter of 50% H3O2P can be obtained for as little as $14.10.

One chemical supply house in Southern California is reported to have sold H3O2P in containers bearing «Plating Solution» labels. In January 1992, Johnson reported containers of «Plating Solution» to contain a mixture of acids consisting mostly of hydriodic acid [2].

Subsequent to Kern Countys report of H3O2Ps use as a reactant last August, an informal poll of many crime labs in California was made. Most chemists / criminalists have not encountered or recognized H3O2P at a methamphetamine lab investigation. A number of chemists have stated that they actually have observed H3O2P at meth lab scenes, but did not consider it as a reaction ingredient and did not sample it at the time. Others have indicated that they were not aware of its usefulness for manufacturing methamphetamine. Others indicate that it would not be identified in their analytical procedures. Another reported that an unlabeled acidic solution containing phosphorus was retrieved from a scene, but was not characterized further. A 1-gallon sized bottle of H3O2P was found at a clandestine methamphetamine lab fire scene.

Methamphetamine lab scenes using H3O2P have been very common in Australia for a number of years. In 1995, Vallely described its use as a reactant [3]. Skinner discussed the reducing capacity of H3O2P at the 3rd Annual CLIC Seminar at Memphis (1993). Skinner and Oulton presented an analytical technique for the identification of H3O2P at the 5th Annual CLIC Seminar at Colorado Springs (1995).

1. 1. J. Clandestine Laboratory Investigating Chemists Association, Volume 6, Number 4, October 1996, page 13.
   2. J. Clandestine Laboratory Investigating Chemists Association, Volume 2, Number 1, January 1992, page 10.
   3. J. Clandestine Laboratory Investigating Chemists Association, Volume 5, Number 2, April 1995, pages14-15.

Drug Monograph and Reference Manuals

The Association presents a new drug monograph series each year at its Technical Training Seminar.  At the seminar, the monograph is provided to the attendee as part of their registration packet.  The compiler(s) of the monographs present the monograph at the meeting and discuss the organization and content.

The purpose of the monograph is to provide the forensic drug chemist with a concise collection of  the major papers pertaining to a specific drug or drug group.  The Association is pleased to offer these monographs and references to other forensic drug chemists for sale.  A listing of the current monographs and references can be found below.

Please note the manuals are only shipped to forensic laboratories throughout the world on a confirmation basis.  For more information regarding the monographs or to place an order, contact:

Steven B. Johnson Los Angeles PD Crime Lab 555 Ramirez St Ste 270 Los Angeles, CA  90012-6302 (213) 237-0041 – Voice (213) 237-0040 – Fax     Drug Monograph and Reference Titles  Price per set ($US)  Shipping cost ($US)  US  Foreign  A Review of the Synthesis and Analysis of Phenyl-2-propanone, Amphetamine, and Methamphetamine (2 volumes); compiled by
M.F. Kalchik and R.A. Ely, 1993  $35.00  $5.00  $10.00  Structure-Activity Relationships, Synthesis, Precursor Preparation and Analysis of Methylenedioxyamphetamine and Its Analogs and Homologs (4 volumes); compiled by T.A. Dal Cason, 1994  $65.00  $10.00  $15.00  A Review of the Synthesis and Analysis of Phencyclidine and Its Analogs (1 volume); compiled by M.F. Kalchik, 1995  $15.00  $2.50  $7.50  An Analyst’s Guide to the Investigation of Clandestine Laboratories
(1 volume); compiled by K. Weaver and E. Yeung, 1995  $15.00  $2.50  $7.50  A Review of the Synthesis and Analysis of Fentanyl and Its Analogs
(1 volume); compiled by A.C. Allen, 1996  $15.00  $2.50  $7.50