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THE CLANDESTINE LABORATORY INVESTIGATING CHEMISTS ASSOCIATION
CONFERENCE ABSTRACTS FROM
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THE

LATE 1990'S

“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 alphaphenylacetamide. From the chemicals found at the laboratory site, the most likely procedure should have been to first manufacture phenyl-2-propanone 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 phenyl2-propanone 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

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with few exceptions. RCRA has been amended several times. Buntrock and Robert E. TSCA (Toxic Substances Control Act). and sodium acetate. and the available treatment technologies for each.1. Two separate incidents resulting in the deaths of three people in Los Angeles. the Resource Conservation and Recovery Act. or RCRA. Los Angeles. The peculiar twist of this case was that d. 1992-1993” Jerry Massetti. repetitive organized crime type of operation which used the hydriodic acid/red phosphorous reduction of ephedrine to methamphetamine. Los Angeles Police Department Crime Lab. and the necessary inclusion of materials previously unregulated by the Federal Government. Fire and explosion from organic solvents and reactive materials remain a serious threat. and poster graphics. CA 94538 In 1976. The color illustrations were generated on a Hewlett .l-aminorex was not. Additionally. BA. as well as possible alternatives. with the 1984 Hazardous Solid Waste Amendments.l-aminorex is the parent compound of the more conventionally recovered 4-methylaminorex. and Vincent Cordova. The second kind of lab newly observed in Central California in the past year produced hypercin from St. Brown. AIDS cures have occurred in other clandestine drug laboratory investigations in California.. BS. 390 Main Street Room 700. “Fatalities Resulting From Clandestine Drug Manufacturing Laboratories” Roger A. regulatory requirements extend from RCRA (Resource Conservation and Recovery Act). overheads transparencies. Freed. California State Department of Justice. became law.. cyanogen bromide. This presentation discusses the management and disposal options and opportunities in the 1990’s. 2 of 18 9/19/2012 6:53 PM . Included is an overview of the waste streams typical of Clandestine Lab Sites. Fresno Regional Laboratory. Inc.org/archive/rhodium/chemistry/clic. Precursors identified from the laboratory consisted of dl-2-aminolphenylethanol. “Clandestine Aminorex. Findings from street purchases and samples from the lab identified d. Since then. John’s Wort. however. Inc.hydriodic acid reduction of ephedrine can be especially dangerous due to the reactants and byproducts formed from their reaction. One of the scenes corroborated rumors about multiple tons of ephedrine being processed in this way. 6014 North Cedar Avenue. “Disposal Technologies” Jeffrey L. The repetitive aspect of these labs constitute an interesting study in linking sites of serial crimes with physical evidence. PA 19090 In this presentation we describe a case of a fragrance laboratory being used as a cover for clandestine d. The computer graphics were generated on a 486/50 MHz personal computer equipped with 8 MB of RAM. Specific discussion will include examples of disposal facilities of each type. Drug Enforcement Administration. at the time. eliminated the disposal of hazardous waste directly into landfills without previous treatment to specific standards. The system includes a 170 MB IDE hard disk and a super VGA non-interlaced monitor with a BOCA 1 MB video card. This reaction has been used in Central California for years. Management and disposal have been further complicated by State requirements.l-aminorex. Fremont. with regards to clandestine drug wastes. Fresno. d. 4227 Technology Drive. being of the greatest significance. CA. Johnson.The Clandestine Laboratory Investigating Chemists Association . and Steven B.. “Mope Dope and AIDS Cures: Central California Drug Lab Scenes. The first was a highly stylized. a common street drug in the Philadelphia or surrounding east coast area. Ely.[www. and even some pressures from the NRC (Nuclear Regulatory Commission) for management of low-level radioactive materials.. Willow Grove. ID. CA 94105. Western Laboratory. The presentation endeavors to provide an overview of hazardous waste management and disposal as it pertains to Clandestine Drug Lab materials. various solvents. These amendments to RCRA have. One illicit synthetic method to methamphetamine using a red phosphorus . Finally. San Francisco.. and was comprehensive and far-reaching in its impact. a federally controlled Schedule 1 drug. 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. 555 Ramirez Space #270.Packard DeskJet 500C inkjet printer.html formats including slides.erowid. The software used was Computer Support Corporation’s “Arts & Letters” with Windows 3. some innovative variations have streamlined the process. These findings led to the confiscation and dismantling of the laboratory and to the arrest of the suspect involved in producing the d. http://www. or HSWA. will be presented with crime scene reconstructions and postmortem findings. Chemical Waste Management.l-aminorex. 2300 Stratford Avenue. State Programs. A Designer Drug Parent Finds the East Coast” Jason W. 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. This was the first effort on the part of the Federal Government to regulate the management and disposal of hazardous waste. Work with undercover officers throughout a lengthy investigation enabled a search and seizure of the laboratory. National Medical Services. CA 93710 Two new distinctive types of clandestine drug laboratories have been observed in Central California during the last year. and two in Post Falls.l-aminorex laboratory.

this laboratory has received over forty unusual exhibits from Edmonton. Burnaby.erowid. Common examples of its use include taping glass joints and sealing of packages of product or boxes of equipment. “Sodium Bicarbonate Assay in Controlled Substance Exhibits” Thomas R. once formed. Closer inspection of GC-MS data revealed several compounds present in large quantities and appeared to be related to cocaine. undergoes hydrogenolysis to methamphetamine and toluene.[www. Fort Worth. We were able to identify cocaine in some of the samples. 22202 3 of 18 9/19/2012 6:53 PM . “Cocaine in Bleach: Destroying the Evidence. 410 West 35th Street. Forensic Consultant Services. especially in phenethylamines and cocaine. TX 76110 In case after case involving clandestine amphetamine or methamphetamine laboratories. “Examinations of Duct Tape in Clandestine Labs” Max Courtney. B. Alberta. P. Laing. “The Analytical Profiling of Methamphetamine of Various Origins” Peter Fifka. CA 91950 Methamphetamine was synthesized by reductive alkylation hydrogenolysis of phenyl-2-propanone with N-benzylmethylamine. http://www. The reduction of ephedrine using iodine and red phosphorus Prepared samples were examined after previous preconcentration of impurities by GC-MS analysis. 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. Forensic Consultant Services. volumetric analysis can be difficult. It was suspected that the occupants had dumped quantities of cocaine into the bleach for the purpose of destroying the evidence. Identification of Degradation Products” Alexis Carpenter and Richard R.org/archive/rhodium/chemistry/clic. TX 76110 Controlled substance samples occasionally are encountered wherein sodium bicarbonate also is detected. Ekis and Max Courtney. Some compounds were identified among the impurities. Southwest Laboratory. Duct tape offers a wealth of information in comparing questioned and known samples for tying a violator to an offense. Fort Worth. V5G 4P2 In recent months. Arlington. the violators have been seen to employ duct tape. Drug Enforcement Administration. The expected product N-benzylmethamphetamine. the intermediates formed during the reaction. The reductive amination from 1-phenyl-2-propanone and methylamine 2. Police Institute of Criminalistics. 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. Slovakia. VA. but in many others cocaine was totally absent. Drug Analytical Service. National City.. Jiri Zapletal. some of which had traces of cocaine. Banska Bystrica. 3155 Willingdon Green. 97486 Methamphetamine hydrochloride salt has been prepared by two different syntheses: 1.0.Maja 1. Synthesis strategies seem to suggest no logical reason for the presence of bicarbonates in phenethylamines beyond its use as a cutting agent. These exhibits were found to contain liquid bleach. These compounds were identified as degradation products with norcocaine and N-formylcocaine being the most predominant. Health Canada. For either legal or investigative reasons. Richardson. assay of the sodium bicarbonate is sometimes required. and the products were analyzed by gas chromatography and mass spectrometry. PO Box 11668. Health Protection Branch. The progress of the reaction. 9. Box 11668. Drug Enforcement Administration. and Jaromir Novak. Chromatographic spectra of both are different and by the presence of some specific impurities.. The samples were seized during raids on fortified shooting galleries where buckets containing bleach (typically one-gallon ice cream containers) were found.C.The Clandestine Laboratory Investigating Chemists Association . Skinner.. Diversion Control Section. 600 Army-Navy Drive. Due to the buffering properties of the bicarbonate ion.html “Methamphetamine Synthesis Via Reductive Alkylation Hydrogenolysis of Phenyl-2-Propanone with N-Benzylmethylamine” Harry F. it is possible to determine the way of the synthesis.. Numerous class characteristics and individual characteristics are discussed in this application of criminalistics to the drug enforcement area.

. secluded. http://www.The Clandestine Laboratory Investigating Chemists Association . Sydney. WI). Laing and Brian Dawson. “The Ritter Reaction Using Safrole: An Encounter In Two Clandestine Labs” Richard R. process.3-dimethylrequire H and 6. Australian Government Analytical Laboratory. “An Overview of Central California Clandestine Methamphetamine Laboratories Associated with Mexican Nationals” Jerry Massetti. Kazlauskas and V. San Bernardino County Sheriff’s Crime Laboratory. Aurora Police Department. It is suggested that clandestine lab chemists can use this compound as an indicator of the Ritter or related reactions. although seeming to relate to MDA was partially characterized using IR spectroscopy and mass spectrometry but C NMR techniques for structure confirmation. In repeating the synthesis the desired intermediate N-acetyl MDA was not found at any stage of the reaction. 3155 Willingdon Green. Either ATR or Diffuse Reflectance (DR) can be selected by simply changing the sample holder. BC. Burnaby. 3155 Willingdon Green. V5G 4P2 In two recent MDA clandestine lab seizures. “Secrets of Methamphetamine Manufacture. 92402-0569 The use of hydrogen peroxide in the reduction of ephedrine to methamphetamine has become popular in several western states.. Powders such as cutting agents or methamphetamine can easily be run neat without the preparation of KBr disks in ATR mode. Some manufacturing incidents have aroused environmental impact concerns. acetonitrile and concentrated sulphuric acid are reacted together at cold temperatures. CA 93710 Large capacity clandestine methamphetamine laboratories associated with operatives from Mexico continue to inundate Central California with increasing frequency. B. and places reporting requirements for manufacturers of regulated chemicals. provides administrative authority for regulating drug products containing ingredients used in illicit manufacturing. Pymble. The major product 3.org/archive/rhodium/chemistry/clic. The major reaction product. Madison. “The Use of Hydrogen Peroxide in Ephedrine Reductions: A Growing Trend” Tim McKibben and Troy Ward. Work crews report to remote.C. Laing. and pastes the SplitPea in DR mode affords a wider application and has been applied to routine drug analyses in our laboratory. CA Department of Justice Regional Laboratory. This paper will introduce the use of hydrogen peroxide. Health Canada. and dispose of chemicals and equipment used to manufacture methamphetamine. Seven and ten ton shipments of ephedrine have been documented. 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. An overview of recent cases will be presented. and impurities to the forensic chemist. PO Box 385. Alameda. The new law enhances DEA’s ability to regulate the distribution of certain chemicals used in the illicit manufacture of controlled substances. CA. Aurora. NSW. Health Canada. by analogy to making amphetamine from allybenzene. and Dawn Sorenson. 15001 E. 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. San Bernardino. Fresno. PO Box 569.. Drug Analytical Service. 1704 East Bullard Avenue. “MDA From Safrole by the Ritter Reaction” R. The major product appears to be an isoquinoline.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. Australia. references were found relating to the Ritter reaction in which safrole. Health Protection Branch. 1994. TM TM TM 1 13 4 of 18 9/19/2012 6:53 PM . it gives only a low yield of the expected product. While ATR is primarily used for surface analysis such as films.. Burnaby. Canada V5G 4P2 The SplitPea (Harrick Scientific Corporation.erowid. fibers. usually agricultural sites to discretely deliver. It places more requirements on handlers of these chemicals. The use of peroxide should also be a cause of concern because of its explosive properties. its possible side reactions. FT-IR Micro Sampling ATR Apparatus in Analysis of Drugs of Abuse” “Application of the SplitPea Richard R. N-acetyl MDA. Films and residues on a variety of surfaces can also be analyzed which normally using traditional IR techniques would be very difficult.[www. 80012. 2071 The underground book by Uncle Fester. Murtaugh. The use of this reagent introduces several new possible reaction and byproducts. Health Protection Branch. Ossing.4-dihydro-1.html This presentation will explain the provisions of the federal Domestic Chemical Diversion Control Act of 1993 which became effective on April 16. But when the reaction is applied to safrole and acetonitrile. byproducts. The external sample stage allows facile placement of the sample on the contact surface at the optics focus giving excellent spectra. CO.” mentions use of the Ritter reaction to make MDA from safrole.

Oulton and Harry F. which accounted for 87% of all lab hours. The suspected manufacturing area can be vacuumed and/or methanol wiped and screened immediately at the lab site using the Ionscan. 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. and drug residue being left behind. National City. Most exposures were through inhalation. CA 91950 Clandestine methamphetamine laboratories are prevalent in southern California. Brown and Jeffrey H.South Central Laboratory. or former (equipment removed) labs.org/archive/rhodium/chemistry/clic. cheap and efficient method. 35th Street. CG-09. Albers. Symptoms were primarily those of headache and respiratory/mucous membrane irritation. DEA . because of a World War II patent using these methods.Southwestern Laboratory. 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. 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. Washington Poison Center. Positive results are confirmed by obtaining vacuum sweep samples with subsequent analysis at the DEA laboratory. National City.” Jeffery L. 5 of 18 9/19/2012 6:53 PM . MD. Other routes of synthesis includes the use of hypophosphorus and phosphorus acids coupled with iodine. it poses a significant problem for law enforcement and lab personnel alike.. red phosphorus and water. but one that poses many safety hazards. as it is a very quick. anhydrous ammonia. 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.Southwestern Laboratory. DEA .4% of responses.. Reactions were run several times and yields factors were calculated. these do not reflect the realities occurring in chemical combinations during a synthesis reaction. “The Sodium-Ammonia 'Nazi' Method of Methamphetamine Synthesis” Nick Dawson.75-3.The Clandestine Laboratory Investigating Chemists Association . CA 91950 Laboratory operators typically have chosen the route of synthesis for hydriodic acid by the reaction of iodine.erowid. assumptions were adopted to impose some order and “typicalness” on the situation. http://www.[www. 86% of illnesses occurred during processing. Gender and age were not risk factors for becoming ill. Clandestine hydriodic acid is not typically purified or distilled and therefore an appreciable amount of phosphoric acid is present in the mixture.. This procedure has been utilized successfully for identifying methamphetamine and ephedrine from clandestine laboratories that have been abandoned and/or remodeled. however. in-transit. Burgess. Arkansas 72215 The Missouri and Arkansas region has seen a new clandestine lab method appear in the last two years. 1880 Regal Row. Arkansas State Crime Lab. The most common encountered synthesis results in vapor release. 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. Due to these manufacturing processes. from a commercial source. #3 Natural Resources Drive. Quantitation of hydriodic acid can be estimated utilizing density or accurately quantitated by an acid/base titration. Red Phosphorus And Water” Scott R. Methamphetamine labs accounted for 81-97% of all responses. Skinner. Hydriodic acid prepared commercially is distilled to remove the phosphoric acid. or uncontrolled reactions. Acid samples that contain a mixture of hydriodic acid and an appreciable amount of phosphoric acid are of clandestine origin.O. which utilizes sodium metal. Total illness incident rates varied between 0. Little Rock. Comparin. P. Commercial and clandestine HI can be differentiated and positively identified. phosphoric acid is one of the remaining byproducts. “Illness Reports in Clandestine Drug Laboratory Investigators: A Pilot Study. Box 5371. 35th Street. Termed the “Nazi” method. 410 W. “Application of the Ionscan for the Detection of Methamphetamine and Ephedrine in Abandoned Clandestine Laboratories” Patricia A. 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. 410 W. Dallas. “Identification And Quantitation Of Hydriodic Acid Manufactured From Iodine.html “Estimation of Drug Product Yields from Clandestine Laboratory Synthesis Routes” Edwin G. fire/explosion. DEA . Theoretical yields may be calculated. Seattle. in all probability. and denatured alcohol. and many occurred in the years prior to use of full personal protective equipment. Responding to an active lab carried a 7-15 fold risk of becoming ill as compared with set-up. Acid samples that contain only hydriodic acid are. Each participant completed a questionnaire concerning previous drug lab responses and adverse health effects during response activities.

The role of the private laboratory is one of a check and balance system for the prosecution’s scientific findings. Smith. “Review of Clandestine Laboratories in Northern New Zealand” Rodney J. Alkyl nitrites being supplied for the “adult” market. it is inevitable that defense attorney intervention is close behind..4-methylenedioxyethylamphetamine. Albert Science Centre. Albert Private Bag 92-021.org/archive/rhodium/chemistry/clic. In the absence of an operating methamphetamine laboratory being found in our region. Jr. “Cocaine Processing” John Casale.. Defense attorneys turn to the private sector to miraculously find the solution to the government’s misinterpretation of their clients chemistry curiosity. This presentation will cover some of the approaches taken when working with a seized laboratory already processed by a government crime laboratory. 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.[www. (ESR). or have no response. Norris. specimens collected. Senior Forensic Chemist.. Drug Enforcement Administration. Therefore. VA 22102-3494 The predominant methods currently utilized in South America for illicit production of cocaine are described. and flurazepam. PA 19090 After clandestine drug laboratories are seized. This is done by wiping the tablet onto the clean filter and then screening on the Ionscan. Brown and Pamela R. but contain another substance. the component parts required for the construction. 410 W. In the laboratory they may not have a screening test other than chromatography. DEA . Mt. These include the production of cocaine base from cocaine paste from coca leaf via both the solvent and acid extraction techniques. National Medical Services.html “Screening Of Illicit Tablets Using The Ionscan” Patricia A. 6 of 18 9/19/2012 6:53 PM . 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).The Clandestine Laboratory Investigating Chemists Association . The procedure can also be used to differentiate diazepam. “Bombs And Booby Traps In Clandestine Labs” S/A Alexander F. Hampstead Road. 35th Street. and conversion of cocaine base to cocaine hydrochloride. methaqualone. and as much information as possible regarding each type of lab will be reviewed. Drug Enforcement Administration. Unusual and interesting laboratories have included: MDMA (“Ecstasy”) being manufactured at a will-known alternative community. A review of several clandestine laboratories having different levels of involvement will be discussed. Smith. McLean. MD This workshop will present the recognition and awareness of explosive materials. Baltimore. My laboratory’s involvement will be discussed. CA 91950 Recently. Auckland. Freed. National City. Special Testing and Research Laboratory.Southwestern Laboratory. These tablets either respond the same to field test kits. current “countermeasure” equipment and strategies directed by drug trafficking individuals and organizations to repel law enforcement operations.4-methylenedioxymethamphetamine and 3. or look like one type of tablet. Institute of Environmental Science & Research Ltd. activation. 7704 Old Springhouse Road.erowid. placement. PCP manufacture. and testing complete. This procedure was used to differentiate 3. “Outside Testing Laboratories: Friend or Foe?” Jason W. Willow Grove. This role should not always be viewed as a hostile attack. Mt. a quick screening method is needed to presumptively identify the tablets. Reference materials are provided and the presentation is complemented by extensive slide and video aids. and blast effects of improvised explosive devices. attempts to manufacture methamphetamine will be discussed. both in the field and as evidence submissions. Some interesting literature seized by the police and customs will be illustrated.. the Southwest laboratory has encountered many clandestinely manufactured tablets. http://www. 2300 Stratford Ave.. Many of these tablets are similar in appearance.

Health Canada. http://www. Drug Enforcement Administration.g. U. Eckelmans.erowid.. N-formyl-MDMA) typical for the Leuckart synthesis were also detected. Coos Bay. Drug and Chemical Evaluation Section.html “Clandestine Production Of Amphetamine And Its Analogs: The UK Perspective” Leslie A. Only one tablet with the dove logo was found. several tons of unused precursors were recovered. One of the largest laboratories was raided in 1993. RG7 4PN Seizures of amphetamine and various of its derivatives are increasing at a faster rate than other illicit drugs. they appeared to contain all the necessary equipment for a large scale clandestine laboratory. BC V5G4P2 3 7 of 18 9/19/2012 6:53 PM .000 to $300. and importation/exportation. Aldermaston. he was murdered. C. The confiscated equipment indicated a high degree of sophistication by its operators. two boxes of miscellaneous photographic chemicals were the apparent motive for two “cranksters” to murder their associate. The myth that essential precursors can be extracted from photographic chemicals will be explored. Health Protection Branch. Introduction of increasingly strict precursor controls has forced most production overseas. King. van Haeren. Washington D.org/archive/rhodium/chemistry/clic. B. Impurity profiling has enabled the major sources of amphetamine to be identified. Belgium” V. 600 Army-Navy Drive. but around fifteen clandestine laboratories are found each year. 1988 (1988 Convention). Traces of precursor material (e. the United States must submit specific chemical information to the United Nations on an annual basis: quantities seized. As a party to the 1988 Convention. “Kodak Film Developing Chemicals And Clandestine Methamphetamine Laboratories: An Apparent Motive for Homicide” Katherine S. In the past few years. Ph. OR 97420 On two previous field investigations of clandestine methamphetamine laboratories.D.K.000 if they could just find a cook to extract the precursor chemicals. Office of Diversion Control. National Instituut voor Criminalistiek en Criminologie. Berkshire. and burned up in his new car. Viaene. Wilcox. 333 4th Avenue. most are not controlled by legislation and some present analytical challenges. licit and illicit use. This compound was also identified in the powder discovered in and around the tablet presses and on some of the apparatus. At another site earlier this year.. Laing. seizures by country of origin. Oregon State Police Forensic Laboratory. bottles of Kodak developing solution have been found among the chemicals.. Belgium. Brussels. many new amphetamine analogs have appeared.g. When opened.. “Clandestine Laboratories And Chemical Seizures In The United States and Worldwide” Debbie Wegman. Burnaby. operators were using a 500L steel vessel for production of phenyl-2-propanone. 33 m ) were found in the port of Antwerpen. Chemical analysis with the aid of Gas Chromatography coupled to Mass Spectrometry (GC/MS) techniques revealed the presence of 3. “Cultivation Of Cannabis Seeds Seized From A Retail Store Called ‘HEMP BC’: Examination of THC Purity and Chemical Profiles” Richard R. methods of diversion and illicit manufacture.[www. 20532-0001 The United States is a party to the United Nations Convention against Illicit Traffic in Narcotic Drugs and Psychotropic Substances. “Discovery Of A Clandestine Laboratory In Transit In The Port Of Antwerpen. Belgium Twelve suspicious metal containers (each approx. In this case presentation.4-methylenedioxy-N-methamphetamine (MDMA or XTC). isosafrole) and of chemical intermediates (e. The United States submissions as well as other countries submissions will be discussed. 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. 3155 Willingdon Green.Arescchka. Coppens. When they thought their associate was holding out on them. The murderers thought the photographic chemicals (which were worthless junk) to be worth $250.000 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. Forensic Science Service.C.. and V.The Clandestine Laboratory Investigating Chemists Association . H.

These filters also increase efficiency because "blanks" no longer need to be collected between different samples. However. These towelettes are an inexpensive and viable alternative to carrying solvents to a crime scene.00 a seed. One is based on the classic vacuum sweeping technique and the other is a solvent swabbing technique. hemp flour. Midwest and Eastern US labs reported it by late November.[www. Vancouver City Police raided the storefront and seized numerous quantities of cannabis seeds. In January. Fresno. FL). Their relationship to the development of illicit cocaine signature methods. trace evidence collection and preservation has been closely scrutinized by the courts. “Coca Leaf Alkaloids And Illicit Cocaine Signature” James M. McLean. Contamination of the alcohol may be an issue. California.erowid. At the Drug Enforcement Administration's Western Laboratory in San Francisco. thus requiring "blanks" to be taken before each swabbing. pre-packaged. “Speed Changes: August 1995 – A Lower Gear?” Jerry Massetti. To help identify areas where trace amounts of drugs may be present. Very large amounts of caffeine and nicotinamide were used as diluents. we have successfully used two different procedures to collect trace amounts of drugs. Using clean pre-packaged disposable vacuum filter nozzles solves the issue of sample contamination. cross contamination is possible when collecting trace evidence with a vacuum.. Amphetamine had been a rarity since the mid-1980’s. foodstuffs. and drugs. an instrument known as the Ion Scan has 8 of 18 9/19/2012 6:53 PM . and pre-moistened alcohol towelettes. California State Department of Justice.J. Various types of cannabis seeds were grown under identical conditions in order to determine if the cot per seed reflected the THC concentration. d. These towelettes offer a clean. d. Changes in the physical appearance of samples corresponding to chemical changes were also noticed. fibers. Phenylpropanolamine is being extracted from commercially available tablets such as “AcceleRx Appetite Suppressant” (M. and cannabis seed. d. CA 93710 On August 19. An increasing number of samples were also found to be diluted with dimethylsulfone. 7704 Old Springhouse Road.A. Secondary medicinal compounds like triprolidine and chlorpheniramine carry over into the final clandestinely manufactured products. Carrying methanol for swabbing can be problematic: bottles can break or leak. Casale. and contamination-free way to collect drug residues. Moore and John F. Pinellas Park. Moriwaki.. The vacuum sweep is a classic technique used to collect trace physical evidence such as hairs. 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. http://www. within a few weeks of its first appearance. Fresno Regional Laboratory.l-Amphetamine continues to persist in suspected methamphetamine samples one full year after it first emerged. A solution to the logistic problems of this technique is to use commercially prepared.l-amphetamine and d-methamphetamine mixtures were detected in suspected methamphetamine samples by crime laboratories in at least six Western US states. San Francisco. 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. Simpson trial unfolded. “Mighty Mite”.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.l-Phenylpropanolamine has been substituted for single isomer ephedrine or pseudoephedrine in large scale clandestine laboratories using the hydriodic acid and red phosphorus reduction. DEA – Western Lab. Products. The nozzle head and filter housing must be thoroughly cleaned between each collection. Unfortunately. At the same time as amphetamine appeared.. 6014 North Cedar Avenue. Most activists claim that hemp should have a legitimate place in society and the Hemp BC retail store sells everything from hemp clothing. non-viable cannabis seeds is permitted in bird food while viable seed is illegal. BC there is a strong movement to decriminalize Hemp (Cannabis sativa). the amount of active phenethylamine ingredient dropped dramatically. An alcohol wipe is the second technique we successfully use to collect drug residues at crime scenes and from drug suspects.l-amphetamine began showing up in suspected methamphetamine samples submitted to CA DOJ crime laboratories. and “Thick Gulf Indica” Prices ranged from $1. 1995.org/archive/rhodium/chemistry/clic. Despite this. Amphetamine was present in 14% of approximately 3.html In Vancouver. collecting trace drug evidence can present additional challenges. "Trace Drug Evidence Collection Techniques" William M. compact. The possible contamination and integrity of the evidence are the usual concerns. Under the Narcotic Control Act. VA 22102-3494 Methodology for the isolation and identification of coca leaf alkaloids is described. Most of these seeds were packaged in small numbers and had names such as “Primo Cut”. 1996.50 to $4.The Clandestine Laboratory Investigating Chemists Association . DEA Special Testing and Research Laboratory. d. Federal law restricts carrying quantities of flammable liquids on airline flights. USA Ever since the O.

metal containers were discovered in the Port of Antwerpen. "Possible False Identification of MDEA and Tracing Back Synthetic Pathways in a Clandestine Laboratory" C. 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. From the GC-MS analysis of the material. DEA – Southwestern Laboratory. Areschka and H. especially in southern California. V. Interpretation of the chromatograms and the mass spectrum data revealed that the main peak corresponded to 3. Trace mixtures of ephedrine and pseudoephedrine can be extremely difficult to analyze utilizing common underivatized chromatographic techniques. Belgium Twelve suspicious. other staff chemists assist by providing specialized training in analytical and/or instrumental methodology for particular drugs. and techniques necessary to investigate. "Clandestine Phenethylamine Laboratory Syntheses and Analytical Training" Roger A. Due to their availability. Ely. This mid-polarity phase column effectively separates ephedrine and pseudoephedrine mixtures without having to utilize derivatization techniques. and testify about clandestine phenethylamine laboratories seized in the Western Laboratory's 11-state service area. Since the types of cases and work load vary with each DEA laboratory.erowid. Identification of these compound mixtures can be performed utilizing infrared spectrophotometry. hands-on syntheses and sampling. identification and quantitative analyses procedures.. a written examination and an oral presentation of analytical findings.html been successfully used. skills. This section gives the new chemist the basic knowledge.[www. CA. They contained all the necessary equipment for a clandestine laboratory. San Francisco. 9 of 18 9/19/2012 6:53 PM . the chromatographic and physical separations of these two isomers are difficult.The Clandestine Laboratory Investigating Chemists Association . The program also familiarizes the trainee with the uses and limitations of analytical instrumentation in the Western Laboratory. A second small peak appeared to be 3. The DEA Western Laboratory. Since ephedrine and pseudoephedrine are diastereoisomers. the author has developed and refined the clandestine phenethylamine laboratory investigation and analyses portion of the Western Laboratory's training program. 2. however. A smaller peak was identified as 3. hands-on analytical methodology. van Haeren.4-methylenedioxyamphetamine. which is smaller in the case of MDEA.N-dimethyl-MDA and MDEA are not available. Though one or two "senior" chemists lead the training. combinations of these two precursors are common at laboratory sites. The synthesis route of choice is the reduction of ephedrine or pseudoephedrine with hydriodic acid and red phosphorus.4-methylenedioxy-N-methylamphetamine (MDMA).S. DEA – Western Laboratory. This fact could not be proven directly because commercial standards for N. The unidentified peak is symmetrical.4-methylenedioxy-N-ethylamphetamine (MDEA). and mock court sessions.org/archive/rhodium/chemistry/clic. National Institute of Forensic Science. Coppens. Further examination of the findings. extractions. separation and isolation of ephedrine and pseudoephedrine can be accomplished by simple dry extraction techniques. http://www. except for the signal at m/z= 96. newly hired forensic chemists with the U. USA Clandestine methamphetamine laboratories are prevalent in the United States. it was clear that XTC was produced. Identification can be performed utilizing a gas chromatograph equipped with an HP-50+ column and an infrared detector. whereas the peak corresponding to MDEA gives a slightly more tailing profile due to the NH group in this molecule.N-dimethyl-MDA instead of MDEA. Over the past 5 years. The advantages and disadvantages will be discussed. while no MDEA-TFA can be detected. With sufficient sample size.. San Francisco. "Separation and Identification of Ephedrine and Pseudoephedrine Mixtures" Scott Oulton. 3. Brussels. USA Regardless of their experience in examining suspected controlled substances. 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. National City. Belgium. The training utilizes classroom lecture. Drug Enforcement Administration's (DEA) laboratories must successfully complete a rigorous analytical training program before they are allowed to examine case samples. CA. each laboratory's training program is developed and tailored to suit their needs.. suggests that the second small peak corresponds to N. analyze. This presentation details the clandestine phenethylamine training designed by the author. found in and around the equipment. The following indirect arguments were considered: 1. TFAA derivatization of the found material yields MDMA-TFA and MDA-TFA. The mass spectrum of the unknown substance and MDEA are identical. training introduces the controlled and restricted drug groups including color screening tests.

3 ppm. Generally. In his fourth edition.html This appears to confirm the absence of a NH group in the compound. and this case was no exception. phosphine is seen in the farming industry where it is used as a grain fumigant. dizziness.0 ppm. Drager tubes were used to test for the presence of phosphine gas. Los Angeles. In this presentation some remarks are offered regarding the feasibility of use of the new method for clandestine cooks – based on some Sydney. a more extensive review of scientific literature was conducted. symptomology. Clandestine laboratories are routinely encountered in Los Angeles County and frequently involve crude conditions and poor ventilation. In August of 1996. nausea and vomiting. which was detected at levels in excess of 1. three deceased individuals were discovered in a small motel room in Los Angeles County. Pymble. were contacted. and persons with specific knowledge or experience with phosphine gas.erowid. As no visible signs of injury were apparent on the victims. were noted involving a reaction with phosphorus acid. dyspnea and pulmonary edema are frequently seen. Research has also associated phosphine with possible chromosomal damage and with 10 of 18 9/19/2012 6:53 PM . He now suggests the halo-safrole route. NSW. "Fester Revisited: Comments On Proposed MDMA Synthesis" Vincent Murtagh. 4.The Clandestine Laboratory Investigating Chemists Association .[www. There was concern regarding the exposure of deputies who had initially assessed the scene with no protective equipment to this potentially lethal gas. When MDEA. The Threshold Limit Value is 0. during the manufacturing of methamphetamine. extracted from known MDEA tablets. 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. hydriodic acid and red phosphorus. Australia In the second and third editions of his book. Phosphine is a toxic gas which can be generated during the manufacturing of methamphetamine. Some references however. pain or pressure in the chest.N-dimethyl-MDA was present in the found material. using ephedrine. general toxicity and the chemistry of phosphine gas. due to the phosphine interaction with cytochrome oxidase. This process has been analyzed by various groups and the general view suggests that is not successful for ring-substituted amphetamines. Willers-Russo. colorless gas. USA This paper presents a case involving the death of three individuals suspected to have been overcome by phosphine gas. Most of the scientific literature regarding phosphine exposure deals with the inhalation of the gas by grain fumigators. The primary result at autopsy is generally pulmonary edema. because the correct identification of the by-products of the synthesis of MDMA can help to elucidate the pathways followed in the clandestine production. This conclusion is important. Phosphine (hydrogen phosphide) is a toxic. fatigue. which can be produced by a variety of chemical reactions. In an attempt to adequately address these new concerns." Uncle Fester proposed the Ritter reaction for making MDA. Some studies indicate a correlation between phosphine exposure and the inhibition of electron transport. The symptomology is well documented. "Secrets of Methamphetamine Manufacture. The toxicity of phosphine gas and the symptomology due to inhalation. Australia seizures. Fester agrees. Possible phosphine exposure in the field by criminalists and law enforcement personnel who respond to clandestine laboratories.. Los Angeles County Sheriff's Department. phosphine poisoning was suspected by responding Clandestine Laboratory Task Force personnel. given the type of clandestine labs that we frequently encounter. 2. It has long been known that phosphine can also be generated during the manufacturing of methamphetamine. whose chemical mechanism seems likely. Responding deputies who assessed the scene noted chemicals and glassware consistent with the clandestine manufacture of methamphetamine. 3. CA. Initial review of the standard available reference material revealed little information. "Three Fatalities Involving Phosphine Gas. http://www. The more common symptoms include those involving the lungs and respiratory tract.. was added to the found material. there are no direct references to the generation of phosphine as a by-product.. Although some information about phosphine chemistry is available. These arguments make it highly probable that N. The chemical mechanisms behind the generation of phosphine gas as they relate to the manufacturing of methamphetamine. Other common symptoms include headache. Scientific Services Bureau. Produced as a Result of Methamphetamine Manufacturing" Lynn J. The August 1996 incident raised several concerns and questions regarding lethal exposure. Bronchitis and irritation of the lungs. Australian Government Analytical Labs.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. The presence of N. The objectives of this paper are to discuss: 1.org/archive/rhodium/chemistry/clic. the resultant chromatogram showed that MDEA eluted at a different time than the unidentified peak.

Scientific Investigations Division. high incidence of motorcycle gangs. Scientific Investigation Division. "Bunk Mini–Thins" Gina Williams. The analysis of these inorganic 11 of 18 9/19/2012 6:53 PM .. "Determinations of Cations in Seized Clandestine Laboratory Samples by Capillary Electrophoresis" Victor A.The Clandestine Laboratory Investigating Chemists Association . San Bernardino. DEA – North Central Laboratory. Pills from one lot number contained pseudoephedrine as expected.[www. Analytical data including polarimetry and derivatized gas chromatography used for the enantiomer determination is presented. An attempt has been made to imitate appearance as well as smell. San Bernardino County Sheriff's Dept. The results were surprising in that phosphine was encountered more often than originally suspected. TX. Both types of pills and analytical data are displayed.org/archive/rhodium/chemistry/clic. "Hydrogen Sulfide Fatality" Mahul Anjaria. 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. to the possible hazards of accidental exposure. as no testing for the gas is routinely performed. CA. if any. Pills from the other lot number contained no pseudoephedrine and were not visually similar. Diluent trends in specific areas of the State of Mississippi.. Inside of the room was found a discharging gas cylinder labeled "hydrogen sulfide" which was connected to tubing leading into a bucket of liquid. a Drager pump and tubes for phosphine (as well as a phosphine-specific gas mask) were purchased and utilized in the field. "l-Methamphetamine in the Midwest" Gerald T. MS. college towns. USA Seven exhibits containing l-methamphetamine were analyzed by the DEA – North Central Laboratory early in 1997. USA San Bernardino County Sheriff's seized 100 cases of Mini–Thin tablets bearing two different lot numbers. An APR with organic vapor cartridges was found near the body. USA Many synthesis routes use inorganic components to manufacture illicit drugs. leading to his demise. With respect to possible phosphine exposure from clandestine laboratories it is unknown to what extent. noting any social considerations which could reveal a link between stimulant abuse and each particular county (i. both in the field and in laboratory submissions. Mausolf. when the presence of phosphine might be likely. the "cook" mistakenly used hydrogen sulfide gas instead of hydrogen chloride gas to salt out his finished product. 2. The chemicals used are not controlled and are less hazardous than their genuine counterparts.. USA Recipes for liquids that can imitate "liquid" PCP. San Bernardino County Sheriff's Department. Blaine Kern and Kerri Heward. As a result of this deadly incident. and 3. Once the odor was recognized. The review of this material has led to a better understanding of phosphine. the number of incidents where it was detected increased. and has allowed us to educate our criminalists and other field personnel..). Mississippi Crime Laboratory. USA A deceased male found lying outside of a room which contained a methamphetamine laboratory.. more likely due to the increased awareness than by an increase in the actual number of occurrences. Dallas. and piperidine are given. To illustrate specific county distribution. All bottles were factory labeled and factory sealed. military installations. Concurrent case exhibits containing other controlled as well as non-controlled substances. http://www. "Imitation Liquids for Clandestine Laboratory Investigations" Norman E. Bravenec. Apparently.html Heinz body formation in red blood cells. Skowronski. phenylmagnesium bromide solution. IL. etc.C. Some of the criminalists noted that they had previously encountered the odor before.e. responding personnel are exposed. The primary objectives of this study are: 1. San Bernardino.erowid. DEA – Mid-Atlantic Lab. Washington D. Chicago. Meridian. CA. truck drivers. "A Statistical and Geographic Study of Methamphetamine and Amphetamine Submissions to the Mississippi Crime Laboratory from January 1996 through June 1997" Jamela Naron Johnson. DEA – South Central Laboratory.

Separation of iodide from other anions was achieved by addition of 10% methanol to the background electrolyte. DEA – Southwest Laboratory.75mM hexamethonium hydroxide as an electroosmotic flow modifier. Detection of phosphate anion was observed for the clandestinely prepared HI. San Diego. http://www. CA. magnesium. “Ion Mobility Spectrometry Demonstration” Bryan A. These laboratories have all been associated with a Mexican National style dump site in the Lucerne Valley which was not adequately remediated. Ely. Heward and Ken Lee. be extracted from the dirt on the property in question in significant amounts. short analysis time.. The background electrolyte consisted of 2. solid organics and inorganics. These small ions lack a chromophore so Indirect Photometric Detection (IPD) is employed to obtain detection of these analytes.html components in clandestine laboratory samples can prove to be valuable information in determining the synthesis route used. This workshop will cover the examination of one.The Clandestine Laboratory Investigating Chemists Association . and thorium. CA. USA Anion analysis of hydriodic acid (HI) was conducted using capillary electrophoresis (CE) with indirect photometric detection. San Bernardino County Sheriff's Department. Clandestinely prepared HI made by reacting iodine with phosphorus in water was compared to commercially prepared HI. Henderson. precursors. 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.erowid. San Bernardino. zinc. This workshop will discuss each of the presented extraction methodologies. USA Continuing last year’s presentation – examples will be given to define an analytical scheme based on the pH of solutions found at clandestine laboratory sites. lithium. Analysis of illicit samples of popular synthetic routes will be presented as well as detection of various cations on clandestine glassware and other containers. DEA – Southwestern Laboratory. and 0. San Francisco. The following cations are characterized: aluminum.5cm effective length) x 75m I. Capillary Ion Electrophoresis (CIE) was chosen for the analysis of the cations as it provides good selectivity. whereas commercially prepared HI displayed no detection of phosphate anion. “Clandestine Laboratory Sample Characterization and Extraction Techniques” Roger A. DEA – Southwest Laboratory. nickel.. CONFERENCE WORKSHOPS “Carbonyl and Amine Chemistry: Continued” Harry F. 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. CA. This will include a practical demonstration of this technique in a simulation of field sampling modes. smaller amount of sample (4-7hl). "Anion Analysis of Hydriodic Acid by Capillary Electrophoresis" Nathan Salazar. Scientific Investigations Division. in fact.. Quantitation of iodide was conducted to determine the percent HI in solution with an observed linear dynamic range from 15 to 120 ppm. residues.org/archive/rhodium/chemistry/clic. USA Ion Mobility Spectrometry is a valuable tool in the detection of trace amounts of drugs.7 with sodium hydroxide and triethanolamine. copper. and/or solvents.and two-phase liquids miscible and immiscible with water. lead. and specialized samples such as vacuum pump oils. sodium. 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. CA. DEA – Western Laboratory. The background electrolyte was buffered at pH 7. and provide tips on performing the extractions. An overview of the theory will be offered. Observations and analysis of samples taken by the crime lab show that methamphetamine can. ammonium. chromium.25mM pyromelletic acid as the visualizing agent. CA. San Diego. and equal or lower detection limits (5 to 30 ppb) when compared to ion chromatography or atomic absorption spectrometry. reagents. strontium. Analysis were carried out using a fused silica 70cm (61. capillary at 25°C. liquid samples containing solids. "Dirt Extraction of Methamphetamine" Kerri T. In this workshop. little sample preparation. with 30kV applied potential.[www. San Diego.D. Other topics to be discussed include the 12 of 18 9/19/2012 6:53 PM . potassium. Skinner. mercury. barium. Capillary Ion Electrophoresis is a capillary electrophoresis technique optimized for the rapid determination of low molecular weight inorganic and organic ions. calcium.

Daubert hearing was conducted prior to the criminal trial. This workshop will provide some suggestions and salient points to consider for the clandestine laboratory expert witness. Ely.. The use of court displays cannot be understated. CA.” The purpose of this presentation is to present several ideas on how to prepare these reports. a yield projection at this level was provided. The DEA agents and the local police department put questions to the laboratory as to how much methamphetamine could have been produced. The presentation of often seemingly complex and technical concepts in a manner that a jury or court can understand is a challenge. USA A forensic chemist may not only have to analyze evidentiary samples from a clandestine laboratory. “Frye vs. experience and breadth of knowledge. San Francisco. forensic chemists are required to determine how much more could be made from chemical supplies present at the clandestine laboratory.) Gravimetric Powders Net weight Actual analysis Residue on filter paper Important Reagents When one has a recipe or notes listing the amount of the reagent used for a particular size synthesis batch.. The use of these calculations were challenged and a Frye vs. Testimony regarding clandestine laboratory evidence. computer data. “Production Capacity Reports” Gerald Skrowonski. records (handwritten notes.The Clandestine Laboratory Investigating Chemists Association . USA The ultimate test of the forensic drug chemist’s expertise is in the arena of the court. the production capability has always been calculated as the amount of controlled substance that could be manufactured at the 100% theoretical yield. DEA – North Central Laboratory. In addition. USA The raid on a clandestine laboratory in Park Hills. Cape Girardeau.2]. preparation. yet.html quantitative analysis of methamphetamine and amphetamine by GC-FID. The total amount of drug made can be evaluated from this information 13 of 18 9/19/2012 6:53 PM . These were inventoried. The prosecution decided to utilize these projections in their court case. MO. Chicago. IL. etc. photographed. Daubert: How Much Meth Could A One-Armed Man Cook. LC. This approach has been affirmed by two court decisions [1. processes. Calculations were conducted on how much pseudoephedrine was present and how much methamphetamine could have been produced if the reaction resulted in 100% conversion. The “total amount“ of controlled substance is typically calculated from the samples analyzed in the case. http://www. the identification of the optical isomers of the phenylisopropylamines by derivatization using GC-FID. the values listed may be used.erowid. resulted in the recovery of a number of full and empty pseudoephedrine tablet boxes and bottles.[www. The success or failure of a forensic chemist’s testimony regarding a clandestine laboratory is directly related to the witness’s training. adequate preparation and rehearsal allow the witness to easily convey complicated information in a simple manner. Missouri.org/archive/rhodium/chemistry/clic.. If A One-Armed Man Could Cook” Pamela Johnson. but may also be called upon by prosecutors to prepare a “Production Capacity Report. and reconstructions are very different from the typical controlled substance identification testimony. Since the sodium/ammonia reduction reaction was reported at the time to result in 90% conversion. etc. Occasionally. chemist needs to perform these calculations may be based on: Primary Precursors Tablets Listed Strength Actual analysis Liquids Instrumental techniques (GC. The data that the forensic.) are found at clandestine lab sites indicating past drug production. Semo Regional Crime Lab. DEA – Western Laboratory. “Court Room Presentations” Roger A. and some tips for improving phenethylamine chromatography. and released to the hazardous material disposal unit. Historically.

USA On February 13. One of the individuals arrested was charged with the manufacture of methamphetamine. Indiana State Police. be included in the report..2d 1090 (8th Cir. which can then be subjected to reaction conditions.org/archive/rhodium/chemistry/clic. http://www.[www. while a reasonable percent yield for the particular synthesis employed in the clandestine laboratory is not included in the capacity report. be based on the total amount of “Mexican Drug Trafficking Situation Brief” Robert N.2d 1380./Mexico border. PA. Riverside County District Attorney. This technique is commonly used throughout organic chemistry. El Paso. 96 F. SmithKline Beecham Pharmaceuticals. 1. 884 F. What makes this case unusual is not only that the “cook” was employed by a large pharmaceutical company. 3. “The Kathey James Story” D. “Tryptamines and TIHKAL” Andrew C. Allen. part of a distribution ring dealing in methamphetamine. United State v. The synthesis of DMT and related analogs. Eight individuals. Aurora Police Department. The topics of discussion will include: 1.erowid. 1989) (Maximum amount of methamphetamine that defendant could produce was used in determining base offense level even though defendant inexperienced). was novel in his approach to the manufacture of methamphetamine.. “A Cookers Dream” Eric L. if pertinent. 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. Aurora. Both of these issues will be discussed. Ph. The pharmacology of tryptamine derivatives in terms of structure activity relationships. USA Tryptamines and their significance to forensic science are the subject of this presentation. TX. USA Protecting group chemistry involves the use of reagents to convert a functional group into a “protected” functional group. United States v. Indianapolis. USA An overview of drug-trafficking organizations operating in Mexico and the United States. Animal and botanical sources of tryptamines and related analogs. The future of case law in this area will be discussed and the successes and failures in the legislative arena. were arrested.The Clandestine Laboratory Investigating Chemists Association . The synthesis of indole and substituted indoles. These “protected“ intermediates or precursors have been encountered by forensic chemists and should be familiar to chemists investigating illicit drug manufacturing cases. 4. Evans and Thomas J. Shamanism and its historic role in the use of these hallucinogenics. but.html and. Personalities will be identified. 2. 1997 search warrants were served at two locations southwest of Indianapolis. therefore any calculation must methamphetamine that the defendant was in a position to produce). Lawrence. At the end of this presentation — a taped interview with the “cook” explaining how he made the dope will be viewed. along with a historical perspective of the Mexican Drug Trafficking Organization. 14 of 18 9/19/2012 6:53 PM . John M. Finally. It will also be shown why child endangerment is not a viable theory for criminal liability in a murder trial. 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. Current methodology being utilized by these organizations will be detailed. CA. “Protecting Group Chemistry” Tim McKibben.. Wagner. 6. which would otherwise destroy the unprotected form. and finally. especially in the pharmaceutical industry. Examples of protection group chemistry used in illicit and legal manufacturing will be presented. CO. King of Prussia. Commercial sources of indole analogs as precursors to tryptamine analogs. 2. 1992) (The defendant's purpose here was to manufacture methamphetamine. The location of his lab and the synthesis routes used were unusual.A. This presentation will introduce the forensic chemist to some common protection groups and techniques used to add and remove them from the chemical intermediate.D. Beshore.D. 5.. IN. 1383 (8th Cir. DEA – EPIC – Operational Intelligence Unit.S. Harding. as well as the relationship to criminal organizations operating along the U. Riverside. Davis.

Scientific Investigations Division. “COOK” FAILS CHEM 101. converted to living quarters. Due to the hazardous nature of the environment. indicating that the cylinder was freely discharging.org/archive/rhodium/chemistry/clic.. Forensic Specialist Rice also assisted in photographing the exterior of the scene.000. enter the key figure of Nicholas Sand. Criminalists Mehul B. 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. notes. TEXT On January 30. although the CDL photograph did not particularly resemble the victim. Criminalists Anjaria and Kern donned protective clothing and SCBAs and entered the converted garage. The wallet contained some peso notes and a California Driver's License (CDL). The garage. MDA. Health Canada. Criminalists Anjaria and Kern processed the interior of the garage.The Clandestine Laboratory Investigating Chemists Association . Criminalist. Burnaby. and multimillion-dollar production capacity. and other items commonly associated with the clandestine manufacture of methamphetamine. consistent with the final step of methamphetamine manufacture in which the drug is salted out using hydrogen chloride gas. and ledger sheets all depict a large commercial manufacture and distribution operation. Supervising Criminalist/Deputy Sheriff San Bernardino County Sheriff's Department. additional air cylinder for the SCBAs were requested. multiple identities. red phosphorus. they were directed by Sheriff's Narcotics Detectives to the body of a deceased Hispanic male in his late twenties. The cylinder was connected via tubing to a 5 gallon bucket containing liquid. lye. 4800 gm of MDMA. and DMT in a clandestine lab setting? Answer: Conspiracy. Supervising Criminalist Hiram Evans and Forensic Specialist Karen Rice assisted the Deputy Coroner with an examination of the body of the deceased.. The seized chemicals. and 235 gm of DMT. noting a gas cylinder labeled “hydrogen sulfide” with ice formed on the bottom potion of the cylinder. 200 S Lena Rd. Anjaria and Blaine M. To add intrigue to this case. following a lengthy investigation.html “A Career ‘High’” Richard R. 1997. He had been a fugitive for over 20 years. leading to his demise.866. In the year proceeding the seizure. These sales represented the distribution of 127 gm of LSD. lying supine on the driveway adjacent to what had been the garage. 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. Kern responded to a suspected clandestine drug laboratory in the Muscoy area of San Bernardino. hydriodic acid. Hiram K. CA. the open valve on which he was unable to close. convicted in absentia for the manufacture of LSD. Anjaria.erowid. the records indicated gross wholesale sales in excess of $1. 500 gm of MDA. 15 of 18 9/19/2012 6:53 PM . Laing. international distribution networks. Evans. 1996. San Bernardino. Near the body of the deceased was a half-face air purifying respirator (APR) equipped with organic vapor cartridges.[www. All of these were found in a Vancouver suburban clandestine laboratory that was seized September 26.00.. Canada Question: What do you have when you seize large quantities of LSD. BC. After conferral between the various law enforcement. including rolling set of inked fingerprints and recovery of his wallet. a mop bucket equipped with a press. it was decided to move the body of the deceased upwind from his original position to facilitate the examination of the body. sophisticated laboratory setup. MDMA. fire department and Coroner's representatives. Also present in the building were two-phase liquids. On arrival. located to the rear of the residence. HYDROGEN SULFIDE FATALITY Mehul B. http://www.

as a reaction ingredient at clandestine methamphetamine laboratory scenes. organic vapor. flammable gas having the characteristic. 147. By the way of comparison. Robert E. 2. H O P. Whether the “cook” obtained it on his own or through others is unknown at this time. In those particular instances approximately 25 ml was added to 5 gallons of hydriodic acid (~52-57%. Marion N.html The inked fingerprints of the deceased were submitted to the Lab's Cal-ID unit and subsequently identified as those of a Mexican National. 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.. 300 ppm is immediately dangerous to life and health (IDLH). but in contrast is lighter than air. Dangerous Properties of Industrial Materials. p.. having a characteristic faint odor. Criminalist CA DOJ Crime Lab.org/archive/rhodium/chemistry/clic. as little as fifteen minutes of heat has been applied. p. 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. Merck Index. Fresno. pungent odor of 2 rotten eggs. is employed to contain the ingredients. Reinhold Pub. HYPOPHOSPHOROUS ACID USE INCREASES CLANDESTINE METHAMPHETAMINE LABS Jerry Massetti. Efficiency of the reaction procedure is unclear and has not been established from field observations. and 1000-2000 ppm is usually fatal within minutes [1]. New York. With the sense of smell fatigued. a Kern County criminalist reported H O P was being used to reduce ephedrine at a clandestine 3 2 methamphetamine laboratory scene in that county [1]. it is an insidious irritant and chemical asphyxiant which fatigues the sense of smell..[www. Irving Sax. NJ. heavier than air.. Vapor concentrations as low as 50 ppm in air cause toxic symptoms. 2nd ed. Fatal H S poisoning may occur even more rapidly than 2 following an exposure to similar concentrations of HCN as hydrogen sulfide does not combine with hemoglobin. Since then it has become apparent that H O P is being used 3 2 in most parts of California.” While the odor of hydrogen sulfide is detectable at very low concentrations. Acid gas. Page.. 1996. 1963. with a 50 ppm IDLH level. REFERENCES 1. CA 93710-5856 AT CALIFORNIA With increasing frequency. and Harold N. California crime lab personnel who process clandestine lab scenes are recognizing hypophosphorous acid. 888. those exposed fail to get warning of high concentrations.. Willaims & Wilkins Co. such as a canning jar or a beer bottle. 12th ed. hydrogen cyanide (HCN) is also a colorless. In 3 2 August 1996. This 3 2 large scale reaction using H O P is unusual. 16 of 18 9/19/2012 6:53 PM . MD. The acid is simply poured onto the starting material and iodine crystals. Susan Budavari.The Clandestine Laboratory Investigating Chemists Association . but kills through respiratory paralysis [2]. The great majority of H O P usage has been almost exclusively at "tweeker" league meth labs where 3 2 gram-to-ounce size quantities of product are made at a time. but not the name given on the CDL. Clinical Toxicology of Commerical Products. leading to respiratory paralysis and sudden collapse [3]. and base cartridges generally utilized in APRs are marked to be used with hydrogen sulfide “for escape only. Co. 3. Small disposable glassware. p. Gosselin. Rahway. N. 1704 E.erowid. w/w). flammable gas. Reportedly. 823. No red phosphorous is used. ed. 1957. Hydrogen sulfide (H S) is a colorless. H O P has not been reported to be used as a reactant at large scale 3 2 3 2 (multiple 22 L reaction vessel) methamphetamine laboratories whose investigations commonly associate operatives from Mexico. Gleason... Baltimore. http://www. Bullard. NY. One chemist reported that a 12 liter round bottom flask contained a reaction mixture which utilized H O P.

13. but was not characterized further. One half liter of 50% 3 2 H O P can be obtained for as little as $14. Clandestine Laboratory Investigating Chemists Association. In about a two year period ending December 1996. At the seminar. Skinner discussed the reducing capacity of H O P at the 3rd Annual CLIC 3 2 Seminar at Memphis (1993). 3 2 One chemical supply house in Southern California is reported to have sold H O P in containers bearing "Plating 3 2 Solution" labels. 5.. 2.html Chemical cash sales reported to the California Bureau of Narcotics Enforcement / Clandestine Lab Enforcement Program (BNE / CLEP) corroborate lab scene observations. Subsequent to Kern County’s report of H O P’s use as a reactant last August. Please note the manuals are only shipped to forensic laboratories throughout the world on a confirmation basis. CA 90012-6302 (213) 237-0041 . 2. The Association is pleased to offer these monographs and references to other forensic drug chemists for sale. No 4. Skinner and Oulton presented an analytical technique for the identification of H O P at 3 2 the 5th Annual CLIC Seminar at Colorado Springs (1995).The Clandestine Laboratory Investigating Chemists Association . In 1995. For more information regarding the monographs or to place an order. Johnson Los Angeles PD Crime Lab 555 Ramirez St Ste 270 Los Angeles. DRUG MONOGRAPH AND REFERENCE MANUALS The Association presents a new drug monograph series each year at its Technical Training Seminar.. an informal poll of many crime labs 3 2 in California was made. the monograph is provided to the attendee as part of their registration packet. A 1-gallon sized bottle of H O P was 3 2 found at a clandestine methamphetamine lab fire scene.erowid. J.org/archive/rhodium/chemistry/clic. No 1.10. but did not consider it as a reaction ingredient and did not sample it at the time. In January 1992. 6. 3 2 Vallely described its use as a reactant [3]. pp. p.383. The compiler(s) of the monographs present the monograph at the meeting and discuss the organization and content. Johnson reported containers of "Plating Solution" to contain a mixture of acids consisting mostly of hydriodic acid [2]. p. J. Vol. January 1992. Methamphetamine lab scenes using H O P have been very common in Australia for a number of years. A listing of the current monographs and references can be found below. April 1995. Clandestine Laboratory Investigating Chemists Association. A number of chemists have stated that they actually have observed H O P at 3 2 meth lab scenes.Fax Drug Monograph and Reference Titles Shipping cost Price (per set) US Foreign 17 of 18 9/19/2012 6:53 PM . Cash sales of chemicals in California exceeding one hundred dollars are required to be reported to BNE/CLEP. 14-15.Voice (213) 237-0040 .844 to $60. Vol. Clandestine Laboratory Investigating Chemists Association.[www. Most chemists / criminalists have not encountered or recognized H O P at a 3 2 methamphetamine lab investigation. 1. Others have indicated that they were not aware of its usefulness for manufacturing methamphetamine. J.. Vol. http://www. 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. Another reported that an unlabeled acidic solution containing phosphorus was retrieved from a scene. contact: Steven B. No 2. the amount of H O P reported to this program has more than tripled from $18. Others indicate that it would not be identified in their analytical procedures. 3. 10. October 1996.

A.erowid. and Methamphetamine(2 volumes). compiled by K. Ely. 1995 $35.The Clandestine Laboratory Investigating Chemists Association .50 $7.C.00 $10. Weaver and E.. Allen. 1994 A Review of the Synthesis and Analysis of Phencyclidine and Its Analogs (1 volume). Kalchik. compiled by M.00 (1 volume).50 $2.50 $7. http://www.00 $15.org/archive/rhodium/chemistry/clic. Precursor Preparation and Analysis of Methylenedioxyamphetamine and Its Analogs and Homologs(4 volumes).00 $10. Synthesis.. 1996 18 of 18 9/19/2012 6:53 PM .00 $5. Kalchik and R.F. compiled by A.00 $15. 1995 A Review of the Synthesis and Analysis of Fentanyl and Its Analogs $15..00 $65.A.F. compiled by M. Amphetamine.[www.50 $7.50 An Analyst’s Guide to the Investigation of Clandestine Laboratories $15. compiled by T. 1993 Structure-Activity Relationships. Yeung.html A Review of the Synthesis and Analysis of Phenyl-2-propanone.50 $2.00 $2. Dal Cason.00 (1 volume).