The Clandestine Laboratory Investigating Chemists Association - [www....http://www.erowid.org/archive/rhodium/chemistry/clic.html This file is a part of the Rhodium site archive. This Aug 2004 static snapshot is hosted by Erowid as of May 2005 and is not being updated. > > Back to Rhodium Archive Index > > [WWW.RHODIUM.WS] [] [CHEMISTRY ARCHIVE] THE CLANDESTINE LABORATORY INVESTIGATING CHEMISTS ASSOCIATION CONFERENCE ABSTRACTS FROM HTML by Rhodium 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 1 of 18 9/19/2012 6:53 PM the Resource Conservation and Recovery Act. “Disposal Technologies” Jeffrey L. as well as possible alternatives. Ely. cyanogen bromide. Included is an overview of the waste streams typical of Clandestine Lab Sites. Fresno Regional Laboratory. Freed. Work with undercover officers throughout a lengthy investigation enabled a search and seizure of the laboratory. Chemical Waste Management. Drug Enforcement Administration. These amendments to RCRA have. California State Department of Justice.. and was comprehensive and far-reaching in its impact. overheads transparencies. The first was a highly stylized. with the 1984 Hazardous Solid Waste Amendments. TSCA (Toxic Substances Control Act). and Vincent Cordova.[www.erowid. repetitive organized crime type of operation which used the hydriodic acid/red phosphorous reduction of ephedrine to methamphetamine. and the available treatment technologies for each. PA 19090 In this presentation we describe a case of a fragrance laboratory being used as a cover for clandestine d. Management and disposal have been further complicated by State requirements. This presentation discusses the management and disposal options and opportunities in the 1990’s. The software used was Computer Support Corporation’s “Arts & Letters” with Windows 3. San Francisco. Los Angeles Police Department Crime Lab. “Mope Dope and AIDS Cures: Central California Drug Lab Scenes. 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. and Steven B.l-aminorex is the parent compound of the more conventionally recovered 4-methylaminorex. RCRA has been amended several times. and poster graphics. A Designer Drug Parent Finds the East Coast” Jason W. at the time. Inc. regulatory requirements extend from RCRA (Resource Conservation and Recovery Act).. Brown.1.The Clandestine Laboratory Investigating Chemists Association . ID. with few exceptions. Johnson. John’s Wort. will be presented with crime scene reconstructions and postmortem findings. 4227 Technology Drive. Finally. AIDS cures have occurred in other clandestine drug laboratory investigations in California. Los Angeles. d. 2 of 18 9/19/2012 6:53 PM . Fire and explosion from organic solvents and reactive materials remain a serious threat. CA. Precursors identified from the laboratory consisted of dl-2-aminolphenylethanol. The peculiar twist of this case was that d. Fremont. 2300 Stratford Avenue. The second kind of lab newly observed in Central California in the past year produced hypercin from St. These findings led to the confiscation and dismantling of the laboratory and to the arrest of the suspect involved in producing the d. and even some pressures from the NRC (Nuclear Regulatory Commission) for management of low-level radioactive materials. This was the first effort on the part of the Federal Government to regulate the management and disposal of hazardous waste.Packard DeskJet 500C inkjet printer. and two in Post Falls. State Programs.hydriodic acid reduction of ephedrine can be especially dangerous due to the reactants and byproducts formed from their reaction.l-aminorex laboratory. Inc. CA 94538 In 1976. Fresno. CA 94105. Findings from street purchases and samples from the lab identified d. “Clandestine Aminorex. Since then. BS.html formats including slides. or HSWA. http://www. Specific discussion will include examples of disposal facilities of each type. being of the greatest significance. 390 Main Street Room 700. however..l-aminorex. Willow Grove.l-aminorex. Two separate incidents resulting in the deaths of three people in Los Angeles. One illicit synthetic method to methamphetamine using a red phosphorus . The computer graphics were generated on a 486/50 MHz personal computer equipped with 8 MB of RAM. became law. with regards to clandestine drug wastes. a common street drug in the Philadelphia or surrounding east coast area. 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. Buntrock and Robert E. The color illustrations were generated on a Hewlett . CA 93710 Two new distinctive types of clandestine drug laboratories have been observed in Central California during the last year. some innovative variations have streamlined the process. The repetitive aspect of these labs constitute an interesting study in linking sites of serial crimes with physical evidence.org/archive/rhodium/chemistry/clic. One of the scenes corroborated rumors about multiple tons of ephedrine being processed in this way.. 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. BA. and the necessary inclusion of materials previously unregulated by the Federal Government.l-aminorex was not. a federally controlled Schedule 1 drug. eliminated the disposal of hazardous waste directly into landfills without previous treatment to specific standards. National Medical Services. This reaction has been used in Central California for years.. Additionally. 6014 North Cedar Avenue. “Fatalities Resulting From Clandestine Drug Manufacturing Laboratories” Roger A. 1992-1993” Jerry Massetti. and sodium acetate. or RCRA. 555 Ramirez Space #270. The system includes a 170 MB IDE hard disk and a super VGA non-interlaced monitor with a BOCA 1 MB video card. Banska Bystrica. Numerous class characteristics and individual characteristics are discussed in this application of criminalistics to the drug enforcement area. Southwest Laboratory. Closer inspection of GC-MS data revealed several compounds present in large quantities and appeared to be related to cocaine. Richardson. National City. The expected product N-benzylmethamphetamine. Police Institute of Criminalistics. undergoes hydrogenolysis to methamphetamine and toluene. The reduction of ephedrine using iodine and red phosphorus Prepared samples were examined after previous preconcentration of impurities by GC-MS analysis. The samples were seized during raids on fortified shooting galleries where buckets containing bleach (typically one-gallon ice cream containers) were found. Arlington. P.C.erowid. Common examples of its use include taping glass joints and sealing of packages of product or boxes of equipment. 3155 Willingdon Green.. Forensic Consultant Services.The Clandestine Laboratory Investigating Chemists Association . 410 West 35th Street.html “Methamphetamine Synthesis Via Reductive Alkylation Hydrogenolysis of Phenyl-2-Propanone with N-Benzylmethylamine” Harry F.0. the violators have been seen to employ duct tape. 9. TX 76110 Controlled substance samples occasionally are encountered wherein sodium bicarbonate also is detected. Drug Enforcement Administration. Alberta. Box 11668. The progress of the reaction.. assay of the sodium bicarbonate is sometimes required. The reductive amination from 1-phenyl-2-propanone and methylamine 2. but in many others cocaine was totally absent. 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. “Cocaine in Bleach: Destroying the Evidence. We were able to identify cocaine in some of the samples. once formed.org/archive/rhodium/chemistry/clic. and Jaromir Novak. “Sodium Bicarbonate Assay in Controlled Substance Exhibits” Thomas R. Burnaby. TX 76110 In case after case involving clandestine amphetamine or methamphetamine laboratories. some of which had traces of cocaine..[www.Maja 1. Fort Worth. CA 91950 Methamphetamine was synthesized by reductive alkylation hydrogenolysis of phenyl-2-propanone with N-benzylmethylamine. “The Domestic Chemical Diversion Control Act of 1993” Clyde F. For either legal or investigative reasons. 22202 3 of 18 9/19/2012 6:53 PM . Due to the buffering properties of the bicarbonate ion. Drug Analytical Service. Synthesis strategies seem to suggest no logical reason for the presence of bicarbonates in phenethylamines beyond its use as a cutting agent. Some compounds were identified among the impurities. Fort Worth. Jiri Zapletal. and the products were analyzed by gas chromatography and mass spectrometry. 97486 Methamphetamine hydrochloride salt has been prepared by two different syntheses: 1. Skinner. It was suspected that the occupants had dumped quantities of cocaine into the bleach for the purpose of destroying the evidence. the intermediates formed during the reaction. “Examinations of Duct Tape in Clandestine Labs” Max Courtney. 600 Army-Navy Drive. These exhibits were found to contain liquid bleach. Chromatographic spectra of both are different and by the presence of some specific impurities. http://www. Ekis and Max Courtney. Laing. Duct tape offers a wealth of information in comparing questioned and known samples for tying a violator to an offense. Forensic Consultant Services. it is possible to determine the way of the synthesis. Health Canada. Health Protection Branch.. This presentation deals with the methodology of titration and the selection of proper endpoint indicators suitable for titration of bicarbonates. These compounds were identified as degradation products with norcocaine and N-formylcocaine being the most predominant. this laboratory has received over forty unusual exhibits from Edmonton. PO Box 11668. Drug Enforcement Administration. Slovakia. VA. especially in phenethylamines and cocaine. B. V5G 4P2 In recent months. Identification of Degradation Products” Alexis Carpenter and Richard R. Diversion Control Section. volumetric analysis can be difficult. “The Analytical Profiling of Methamphetamine of Various Origins” Peter Fifka. 1704 East Bullard Avenue. Australia. Laing and Brian Dawson.. N-acetyl MDA. 92402-0569 The use of hydrogen peroxide in the reduction of ephedrine to methamphetamine has become popular in several western states. The major product appears to be an isoquinoline. B.” mentions use of the Ritter reaction to make MDA from safrole. “The Ritter Reaction Using Safrole: An Encounter In Two Clandestine Labs” Richard R. Aurora Police Department. Burnaby. Fresno. Seven and ten ton shipments of ephedrine have been documented. and pastes the SplitPea in DR mode affords a wider application and has been applied to routine drug analyses in our laboratory. http://www. The major product 3. In repeating the synthesis the desired intermediate N-acetyl MDA was not found at any stage of the reaction. “The Use of Hydrogen Peroxide in Ephedrine Reductions: A Growing Trend” Tim McKibben and Troy Ward. CA. 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. This paper will introduce the use of hydrogen peroxide. and places reporting requirements for manufacturers of regulated chemicals. Powders such as cutting agents or methamphetamine can easily be run neat without the preparation of KBr disks in ATR mode. Aurora. The major reaction product. although seeming to relate to MDA was partially characterized using IR spectroscopy and mass spectrometry but C NMR techniques for structure confirmation. Ossing. 15001 E.. Pymble. Some manufacturing incidents have aroused environmental impact concerns. and impurities to the forensic chemist. 2071 The underground book by Uncle Fester. CO. But when the reaction is applied to safrole and acetonitrile. Madison. Health Protection Branch.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... references were found relating to the Ritter reaction in which safrole. process. and Dawn Sorenson. TM TM TM 1 13 4 of 18 9/19/2012 6:53 PM . Laing.html This presentation will explain the provisions of the federal Domestic Chemical Diversion Control Act of 1993 which became effective on April 16. BC. It is suggested that clandestine lab chemists can use this compound as an indicator of the Ritter or related reactions. and dispose of chemicals and equipment used to manufacture methamphetamine. The external sample stage allows facile placement of the sample on the contact surface at the optics focus giving excellent spectra. Health Canada. CA Department of Justice Regional Laboratory. The use of this reagent introduces several new possible reaction and byproducts. usually agricultural sites to discretely deliver. Burnaby.C.[www.erowid. “MDA From Safrole by the Ritter Reaction” R.3-dimethylrequire H and 6. 3155 Willingdon Green. An overview of recent cases will be presented. PO Box 385. 1994. by analogy to making amphetamine from allybenzene. byproducts. PO Box 569. San Bernardino. “An Overview of Central California Clandestine Methamphetamine Laboratories Associated with Mexican Nationals” Jerry Massetti. Sydney. Work crews report to remote. secluded. The use of peroxide should also be a cause of concern because of its explosive properties. provides administrative authority for regulating drug products containing ingredients used in illicit manufacturing. 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. WI). Alameda. 80012. acetonitrile and concentrated sulphuric acid are reacted together at cold temperatures. Kazlauskas and V. Health Canada. 3155 Willingdon Green. Murtaugh. NSW. Australian Government Analytical Laboratory. Health Protection Branch.4-dihydro-1. Either ATR or Diffuse Reflectance (DR) can be selected by simply changing the sample holder. V5G 4P2 In two recent MDA clandestine lab seizures. CA 93710 Large capacity clandestine methamphetamine laboratories associated with operatives from Mexico continue to inundate Central California with increasing frequency. Films and residues on a variety of surfaces can also be analyzed which normally using traditional IR techniques would be very difficult. it gives only a low yield of the expected product.The Clandestine Laboratory Investigating Chemists Association .org/archive/rhodium/chemistry/clic. “Secrets of Methamphetamine Manufacture. its possible side reactions. While ATR is primarily used for surface analysis such as films. Drug Analytical Service. San Bernardino County Sheriff’s Crime Laboratory. 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. fibers. Canada V5G 4P2 The SplitPea (Harrick Scientific Corporation. FT-IR Micro Sampling ATR Apparatus in Analysis of Drugs of Abuse” “Application of the SplitPea Richard R. No phase of response activities appeared to carry a higher risk of illness after adjusting for total hours. and many occurred in the years prior to use of full personal protective equipment. Skinner. A majority of illness episodes occurred in labs with leak/spills. “The Sodium-Ammonia 'Nazi' Method of Methamphetamine Synthesis” Nick Dawson. The suspected manufacturing area can be vacuumed and/or methanol wiped and screened immediately at the lab site using the Ionscan. National City. assumptions were adopted to impose some order and “typicalness” on the situation. Due to these manufacturing processes. Dallas. 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. Positive results are confirmed by obtaining vacuum sweep samples with subsequent analysis at the DEA laboratory. 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. Gender and age were not risk factors for becoming ill. Termed the “Nazi” method. Arkansas 72215 The Missouri and Arkansas region has seen a new clandestine lab method appear in the last two years. in-transit.4% of responses.html “Estimation of Drug Product Yields from Clandestine Laboratory Synthesis Routes” Edwin G.Southwestern Laboratory. Comparin. Hydriodic acid prepared commercially is distilled to remove the phosphoric acid. “Application of the Ionscan for the Detection of Methamphetamine and Ephedrine in Abandoned Clandestine Laboratories” Patricia A. 5 of 18 9/19/2012 6:53 PM . because of a World War II patent using these methods. Symptoms were primarily those of headache and respiratory/mucous membrane irritation. and drug residue being left behind. #3 Natural Resources Drive. or uncontrolled reactions. 35th Street. red phosphorus and water. DEA . Brown and Jeffrey H. but one that poses many safety hazards.. as it is a very quick. these do not reflect the realities occurring in chemical combinations during a synthesis reaction. it poses a significant problem for law enforcement and lab personnel alike. 410 W. Albers. Red Phosphorus And Water” Scott R. The most common encountered synthesis results in vapor release. and denatured alcohol. Total illness incident rates varied between 0. Arkansas State Crime Lab. which accounted for 87% of all lab hours. Each participant completed a questionnaire concerning previous drug lab responses and adverse health effects during response activities. P.[www. Washington Poison Center. 86% of illnesses occurred during processing. http://www.South Central Laboratory. CA 91950 Laboratory operators typically have chosen the route of synthesis for hydriodic acid by the reaction of iodine. from a commercial source. Reactions were run several times and yields factors were calculated.org/archive/rhodium/chemistry/clic.75-3. Little Rock. Oulton and Harry F. anhydrous ammonia.The Clandestine Laboratory Investigating Chemists Association .O. DEA . National City. 1880 Regal Row. Other routes of synthesis includes the use of hypophosphorus and phosphorus acids coupled with iodine. CA 91950 Clandestine methamphetamine laboratories are prevalent in southern California. Box 5371. Seattle. MD.erowid. DEA . fire/explosion. in all probability. or former (equipment removed) labs. 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. phosphoric acid is one of the remaining byproducts. CG-09.. Clandestine hydriodic acid is not typically purified or distilled and therefore an appreciable amount of phosphoric acid is present in the mixture. 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.. Acid samples that contain a mixture of hydriodic acid and an appreciable amount of phosphoric acid are of clandestine origin. Methamphetamine labs accounted for 81-97% of all responses. Responding to an active lab carried a 7-15 fold risk of becoming ill as compared with set-up. 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. which utilizes sodium metal. This procedure has been utilized successfully for identifying methamphetamine and ephedrine from clandestine laboratories that have been abandoned and/or remodeled. Most exposures were through inhalation. Commercial and clandestine HI can be differentiated and positively identified.Southwestern Laboratory. Burgess. “Identification And Quantitation Of Hydriodic Acid Manufactured From Iodine. 35th Street. Theoretical yields may be calculated. however. 410 W. Quantitation of hydriodic acid can be estimated utilizing density or accurately quantitated by an acid/base titration. “Illness Reports in Clandestine Drug Laboratory Investigators: A Pilot Study. cheap and efficient method. Acid samples that contain only hydriodic acid are.” Jeffery L. DEA . 6 of 18 9/19/2012 6:53 PM . Smith. Jr.. My laboratory’s involvement will be discussed. National City. McLean. A review of several clandestine laboratories having different levels of involvement will be discussed. activation. 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 procedure was used to differentiate 3.. Norris. Hampstead Road. Mt. Senior Forensic Chemist. 2300 Stratford Ave.4-methylenedioxyethylamphetamine. This role should not always be viewed as a hostile attack. Smith. Brown and Pamela R. These include the production of cocaine base from cocaine paste from coca leaf via both the solvent and acid extraction techniques. This presentation will cover some of the approaches taken when working with a seized laboratory already processed by a government crime laboratory. Therefore.org/archive/rhodium/chemistry/clic. and blast effects of improvised explosive devices.. In the laboratory they may not have a screening test other than chromatography. MD This workshop will present the recognition and awareness of explosive materials. the Southwest laboratory has encountered many clandestinely manufactured tablets. In the absence of an operating methamphetamine laboratory being found in our region.html “Screening Of Illicit Tablets Using The Ionscan” Patricia A. Alkyl nitrites being supplied for the “adult” market. a quick screening method is needed to presumptively identify the tablets. Auckland. and conversion of cocaine base to cocaine hydrochloride. Albert Private Bag 92-021. methaqualone. http://www. specimens collected. or have no response. Unusual and interesting laboratories have included: MDMA (“Ecstasy”) being manufactured at a will-known alternative community. (ESR).[www. Institute of Environmental Science & Research Ltd. “Outside Testing Laboratories: Friend or Foe?” Jason W. but contain another substance.4-methylenedioxymethamphetamine and 3. Freed. PA 19090 After clandestine drug laboratories are seized.The Clandestine Laboratory Investigating Chemists Association .. This is done by wiping the tablet onto the clean filter and then screening on the Ionscan. 35th Street. and as much information as possible regarding each type of lab will be reviewed. or look like one type of tablet. “Cocaine Processing” John Casale. current “countermeasure” equipment and strategies directed by drug trafficking individuals and organizations to repel law enforcement operations.. and testing complete. 7704 Old Springhouse Road. 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 procedure can also be used to differentiate diazepam. Willow Grove. Drug Enforcement Administration. “Review of Clandestine Laboratories in Northern New Zealand” Rodney J.Southwestern Laboratory. The role of the private laboratory is one of a check and balance system for the prosecution’s scientific findings. Defense attorneys turn to the private sector to miraculously find the solution to the government’s misinterpretation of their clients chemistry curiosity. attempts to manufacture methamphetamine will be discussed. VA 22102-3494 The predominant methods currently utilized in South America for illicit production of cocaine are described. “Bombs And Booby Traps In Clandestine Labs” S/A Alexander F. Reference materials are provided and the presentation is complemented by extensive slide and video aids. both in the field and as evidence submissions. Some interesting literature seized by the police and customs will be illustrated. and flurazepam. placement. it is inevitable that defense attorney intervention is close behind. Many of these tablets are similar in appearance. These tablets either respond the same to field test kits. Albert Science Centre. PCP manufacture. Mt. Special Testing and Research Laboratory. Drug Enforcement Administration.erowid. Baltimore. the component parts required for the construction. National Medical Services. CA 91950 Recently. 410 W. 000 if they could just find a cook to extract the precursor chemicals. Drug Enforcement Administration.. Brussels. Laing. U. BC V5G4P2 3 7 of 18 9/19/2012 6:53 PM . National Instituut voor Criminalistiek en Criminologie. Chemical analysis with the aid of Gas Chromatography coupled to Mass Spectrometry (GC/MS) techniques revealed the presence of 3. most are not controlled by legislation and some present analytical challenges.[www.erowid. OR 97420 On two previous field investigations of clandestine methamphetamine laboratories. Wilcox. Impurity profiling has enabled the major sources of amphetamine to be identified.000 to $300. 600 Army-Navy Drive. operators were using a 500L steel vessel for production of phenyl-2-propanone.Arescchka. http://www. bottles of Kodak developing solution have been found among the chemicals.. 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.D. Belgium” V. and V. isosafrole) and of chemical intermediates (e. van Haeren. Aldermaston.. When they thought their associate was holding out on them.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. “Cultivation Of Cannabis Seeds Seized From A Retail Store Called ‘HEMP BC’: Examination of THC Purity and Chemical Profiles” Richard R. The United States submissions as well as other countries submissions will be discussed. This compound was also identified in the powder discovered in and around the tablet presses and on some of the apparatus. but around fifteen clandestine laboratories are found each year. Coos Bay. N-formyl-MDMA) typical for the Leuckart synthesis were also detected. Burnaby. When opened. The confiscated equipment indicated a high degree of sophistication by its operators. In this case presentation. King. several tons of unused precursors were recovered. C. In the past few years. Drug and Chemical Evaluation Section. Oregon State Police Forensic Laboratory. Introduction of increasingly strict precursor controls has forced most production overseas. Coppens.g. “Discovery Of A Clandestine Laboratory In Transit In The Port Of Antwerpen. B.g. and importation/exportation. “Clandestine Laboratories And Chemical Seizures In The United States and Worldwide” Debbie Wegman. Only one tablet with the dove logo was found.. and burned up in his new car. Ph. 1988 (1988 Convention). One of the largest laboratories was raided in 1993. At another site earlier this year. “Kodak Film Developing Chemicals And Clandestine Methamphetamine Laboratories: An Apparent Motive for Homicide” Katherine S. Belgium.K. many new amphetamine analogs have appeared.C.. Health Canada. 33 m ) were found in the port of Antwerpen. Health Protection Branch. 3155 Willingdon Green. Forensic Science Service. Viaene. two boxes of miscellaneous photographic chemicals were the apparent motive for two “cranksters” to murder their associate. Washington D. RG7 4PN Seizures of amphetamine and various of its derivatives are increasing at a faster rate than other illicit drugs. Office of Diversion Control.org/archive/rhodium/chemistry/clic. Traces of precursor material (e. As a party to the 1988 Convention. The myth that essential precursors can be extracted from photographic chemicals will be explored. he was murdered.html “Clandestine Production Of Amphetamine And Its Analogs: The UK Perspective” Leslie A. 20532-0001 The United States is a party to the United Nations Convention against Illicit Traffic in Narcotic Drugs and Psychotropic Substances. 333 4th Avenue.4-methylenedioxy-N-methamphetamine (MDMA or XTC). H. Berkshire. licit and illicit use. seizures by country of origin. Eckelmans.The Clandestine Laboratory Investigating Chemists Association . The murderers thought the photographic chemicals (which were worthless junk) to be worth $250. Belgium Twelve suspicious metal containers (each approx. methods of diversion and illicit manufacture. they appeared to contain all the necessary equipment for a large scale clandestine laboratory. the United States must submit specific chemical information to the United Nations on an annual basis: quantities seized. Carrying methanol for swabbing can be problematic: bottles can break or leak. To help identify areas where trace amounts of drugs may be present. Contamination of the alcohol may be an issue. BC there is a strong movement to decriminalize Hemp (Cannabis sativa). Despite this. California. non-viable cannabis seeds is permitted in bird food while viable seed is illegal. Federal law restricts carrying quantities of flammable liquids on airline flights. Products. trace evidence collection and preservation has been closely scrutinized by the courts. within a few weeks of its first appearance. FL). Secondary medicinal compounds like triprolidine and chlorpheniramine carry over into the final clandestinely manufactured products. an instrument known as the Ion Scan has 8 of 18 9/19/2012 6:53 PM . DEA – Western Lab. 1996. Casale. DEA Special Testing and Research Laboratory. Using clean pre-packaged disposable vacuum filter nozzles solves the issue of sample contamination. Various types of cannabis seeds were grown under identical conditions in order to determine if the cot per seed reflected the THC concentration. VA 22102-3494 Methodology for the isolation and identification of coca leaf alkaloids is described. USA Ever since the O.A. compact. Pinellas Park. One is based on the classic vacuum sweeping technique and the other is a solvent swabbing technique. foodstuffs..erowid. http://www. These towelettes offer a clean. pre-packaged. d.org/archive/rhodium/chemistry/clic. At the same time as amphetamine appeared.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. 1995. Amphetamine was present in 14% of approximately 3. Very large amounts of caffeine and nicotinamide were used as diluents. California State Department of Justice. However. A solution to the logistic problems of this technique is to use commercially prepared. McLean. 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. Amphetamine had been a rarity since the mid-1980’s. These towelettes are an inexpensive and viable alternative to carrying solvents to a crime scene. CA 93710 On August 19.00 a seed. d.l-amphetamine and d-methamphetamine mixtures were detected in suspected methamphetamine samples by crime laboratories in at least six Western US states.. Vancouver City Police raided the storefront and seized numerous quantities of cannabis seeds. Fresno. An increasing number of samples were also found to be diluted with dimethylsulfone. At the Drug Enforcement Administration's Western Laboratory in San Francisco. “Coca Leaf Alkaloids And Illicit Cocaine Signature” James M.l-Phenylpropanolamine has been substituted for single isomer ephedrine or pseudoephedrine in large scale clandestine laboratories using the hydriodic acid and red phosphorus reduction. fibers. Simpson trial unfolded.l-amphetamine began showing up in suspected methamphetamine samples submitted to CA DOJ crime laboratories.. San Francisco. 7704 Old Springhouse Road. and contamination-free way to collect drug residues. cross contamination is possible when collecting trace evidence with a vacuum. d. Most activists claim that hemp should have a legitimate place in society and the Hemp BC retail store sells everything from hemp clothing. In January. An alcohol wipe is the second technique we successfully use to collect drug residues at crime scenes and from drug suspects. Unfortunately. “Speed Changes: August 1995 – A Lower Gear?” Jerry Massetti. 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. Moore and John F.l-Amphetamine continues to persist in suspected methamphetamine samples one full year after it first emerged.The Clandestine Laboratory Investigating Chemists Association .html In Vancouver. we have successfully used two different procedures to collect trace amounts of drugs. The nozzle head and filter housing must be thoroughly cleaned between each collection. These filters also increase efficiency because "blanks" no longer need to be collected between different samples. Midwest and Eastern US labs reported it by late November. Moriwaki. and drugs.J. Their relationship to the development of illicit cocaine signature methods. the amount of active phenethylamine ingredient dropped dramatically.50 to $4. Under the Narcotic Control Act. The possible contamination and integrity of the evidence are the usual concerns.[www. and pre-moistened alcohol towelettes. thus requiring "blanks" to be taken before each swabbing. and cannabis seed. Most of these seeds were packaged in small numbers and had names such as “Primo Cut”. d. and “Thick Gulf Indica” Prices ranged from $1. Changes in the physical appearance of samples corresponding to chemical changes were also noticed. "Trace Drug Evidence Collection Techniques" William M. Fresno Regional Laboratory. collecting trace drug evidence can present additional challenges. hemp flour. The vacuum sweep is a classic technique used to collect trace physical evidence such as hairs. Phenylpropanolamine is being extracted from commercially available tablets such as “AcceleRx Appetite Suppressant” (M. 6014 North Cedar Avenue. “Mighty Mite”. Belgium Twelve suspicious.. which is smaller in the case of MDEA. TFAA derivatization of the found material yields MDMA-TFA and MDA-TFA. The synthesis route of choice is the reduction of ephedrine or pseudoephedrine with hydriodic acid and red phosphorus. newly hired forensic chemists with the U. while no MDEA-TFA can be detected. and testify about clandestine phenethylamine laboratories seized in the Western Laboratory's 11-state service area. 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. Identification can be performed utilizing a gas chromatograph equipped with an HP-50+ column and an infrared detector. DEA – Southwestern Laboratory. CA. combinations of these two precursors are common at laboratory sites. The advantages and disadvantages will be discussed.S. a written examination and an oral presentation of analytical findings. Identification of these compound mixtures can be performed utilizing infrared spectrophotometry. whereas the peak corresponding to MDEA gives a slightly more tailing profile due to the NH group in this molecule. "Possible False Identification of MDEA and Tracing Back Synthetic Pathways in a Clandestine Laboratory" C. training introduces the controlled and restricted drug groups including color screening tests. Since ephedrine and pseudoephedrine are diastereoisomers. The following indirect arguments were considered: 1. separation and isolation of ephedrine and pseudoephedrine can be accomplished by simple dry extraction techniques. hands-on analytical methodology.html been successfully used. 3. especially in southern California. Though one or two "senior" chemists lead the training.[www. USA Regardless of their experience in examining suspected controlled substances. hands-on syntheses and sampling. found in and around the equipment. except for the signal at m/z= 96. A second small peak appeared to be 3. This mid-polarity phase column effectively separates ephedrine and pseudoephedrine mixtures without having to utilize derivatization techniques. metal containers were discovered in the Port of Antwerpen. each laboratory's training program is developed and tailored to suit their needs. Belgium. National City. With sufficient sample size..The Clandestine Laboratory Investigating Chemists Association . National Institute of Forensic Science.4-methylenedioxy-N-ethylamphetamine (MDEA). This fact could not be proven directly because commercial standards for N. Over the past 5 years. The mass spectrum of the unknown substance and MDEA are identical. 2. Coppens. CA. From the GC-MS analysis of the material. They contained all the necessary equipment for a clandestine laboratory. suggests that the second small peak corresponds to N.. skills.4-methylenedioxy-N-methylamphetamine (MDMA).4-methylenedioxyamphetamine. This presentation details the clandestine phenethylamine training designed by the author. Brussels. V. and mock court sessions. Interpretation of the chromatograms and the mass spectrum data revealed that the main peak corresponded to 3. The training utilizes classroom lecture. however. San Francisco. A smaller peak was identified as 3. USA Clandestine methamphetamine laboratories are prevalent in the United States. This section gives the new chemist the basic knowledge. The program also familiarizes the trainee with the uses and limitations of analytical instrumentation in the Western Laboratory. Drug Enforcement Administration's (DEA) laboratories must successfully complete a rigorous analytical training program before they are allowed to examine case samples. analyze. Due to their availability. "Clandestine Phenethylamine Laboratory Syntheses and Analytical Training" Roger A.N-dimethyl-MDA and MDEA are not available. http://www. van Haeren. Further examination of the findings. it was clear that XTC was produced. "Separation and Identification of Ephedrine and Pseudoephedrine Mixtures" Scott Oulton. The DEA Western Laboratory. 9 of 18 9/19/2012 6:53 PM . DEA – Western Laboratory.erowid. the chromatographic and physical separations of these two isomers are difficult. The unidentified peak is symmetrical. 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. and techniques necessary to investigate.N-dimethyl-MDA instead of MDEA. other staff chemists assist by providing specialized training in analytical and/or instrumental methodology for particular drugs. Areschka and H. identification and quantitative analyses procedures. San Francisco. Since the types of cases and work load vary with each DEA laboratory. Ely.org/archive/rhodium/chemistry/clic. extractions. the author has developed and refined the clandestine phenethylamine laboratory investigation and analyses portion of the Western Laboratory's training program. The more common symptoms include those involving the lungs and respiratory tract. Los Angeles. As no visible signs of injury were apparent on the victims. nausea and vomiting. In an attempt to adequately address these new concerns. He now suggests the halo-safrole route. It has long been known that phosphine can also be generated during the manufacturing of methamphetamine. were noted involving a reaction with phosphorus acid.. Responding deputies who assessed the scene noted chemicals and glassware consistent with the clandestine manufacture of methamphetamine. Pymble. "Fester Revisited: Comments On Proposed MDMA Synthesis" Vincent Murtagh. Australia seizures. which can be produced by a variety of chemical reactions. the resultant chromatogram showed that MDEA eluted at a different time than the unidentified peak. and this case was no exception. USA This paper presents a case involving the death of three individuals suspected to have been overcome by phosphine gas. fatigue. because the correct identification of the by-products of the synthesis of MDMA can help to elucidate the pathways followed in the clandestine production. In August of 1996. Bronchitis and irritation of the lungs. dizziness. using ephedrine. general toxicity and the chemistry of phosphine gas. The Threshold Limit Value is 0. This process has been analyzed by various groups and the general view suggests that is not successful for ring-substituted amphetamines. Australia In the second and third editions of his book..The Clandestine Laboratory Investigating Chemists Association . NSW. were contacted. Other common symptoms include headache. In this presentation some remarks are offered regarding the feasibility of use of the new method for clandestine cooks – based on some Sydney. Fester agrees. Research has also associated phosphine with possible chromosomal damage and with 10 of 18 9/19/2012 6:53 PM . Some references however. This conclusion is important. The symptomology is well documented. The objectives of this paper are to discuss: 1. Most of the scientific literature regarding phosphine exposure deals with the inhalation of the gas by grain fumigators. "Secrets of Methamphetamine Manufacture. Willers-Russo. a more extensive review of scientific literature was conducted. The primary result at autopsy is generally pulmonary edema. was added to the found material. during the manufacturing of methamphetamine. When MDEA. http://www. These arguments make it highly probable that 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. Produced as a Result of Methamphetamine Manufacturing" Lynn J. there are no direct references to the generation of phosphine as a by-product. In his fourth edition. and persons with specific knowledge or experience with phosphine gas. Australian Government Analytical Labs. which was detected at levels in excess of 1. Drager tubes were used to test for the presence of phosphine gas.0 ppm.N-dimethyl-MDA was present in the found material. 3. 2. whose chemical mechanism seems likely. Phosphine (hydrogen phosphide) is a toxic." Uncle Fester proposed the Ritter reaction for making MDA. Although some information about phosphine chemistry is available. phosphine is seen in the farming industry where it is used as a grain fumigant. three deceased individuals were discovered in a small motel room in Los Angeles County. Clandestine laboratories are routinely encountered in Los Angeles County and frequently involve crude conditions and poor ventilation. Phosphine is a toxic gas which can be generated during the manufacturing of methamphetamine..[www. extracted from known MDEA tablets. Generally.org/archive/rhodium/chemistry/clic. Some studies indicate a correlation between phosphine exposure and the inhibition of electron transport. The August 1996 incident raised several concerns and questions regarding lethal exposure.html This appears to confirm the absence of a NH group in the compound. There was concern regarding the exposure of deputies who had initially assessed the scene with no protective equipment to this potentially lethal gas. The presence of N. The chemical mechanisms behind the generation of phosphine gas as they relate to the manufacturing of methamphetamine. This gas is extremely poisonous and can be generated when the reaction mixture is overheated. Scientific Services Bureau. pain or pressure in the chest. Los Angeles County Sheriff's Department. CA. given the type of clandestine labs that we frequently encounter.erowid. Possible phosphine exposure in the field by criminalists and law enforcement personnel who respond to clandestine laboratories. The toxicity of phosphine gas and the symptomology due to inhalation. due to the phosphine interaction with cytochrome oxidase. symptomology. 4. Initial review of the standard available reference material revealed little information. phosphine poisoning was suspected by responding Clandestine Laboratory Task Force personnel. colorless gas. hydriodic acid and red phosphorus. A possible by-product of the ephedrine / hydriodic acid / red phosphorus manufacturing method is phosphine gas. dyspnea and pulmonary edema are frequently seen.3 ppm. "Three Fatalities Involving Phosphine Gas. Apparently. a Drager pump and tubes for phosphine (as well as a phosphine-specific gas mask) were purchased and utilized in the field. Meridian. IL. Mississippi Crime Laboratory.e. An APR with organic vapor cartridges was found near the body. Some of the criminalists noted that they had previously encountered the odor before. truck drivers. An attempt has been made to imitate appearance as well as smell. military installations. phenylmagnesium bromide solution. With respect to possible phosphine exposure from clandestine laboratories it is unknown to what extent. "Bunk Mini–Thins" Gina Williams. As a result of this deadly incident. "Hydrogen Sulfide Fatality" Mahul Anjaria. USA A deceased male found lying outside of a room which contained a methamphetamine laboratory. "Imitation Liquids for Clandestine Laboratory Investigations" Norman E. http://www. San Bernardino. the "cook" mistakenly used hydrogen sulfide gas instead of hydrogen chloride gas to salt out his finished product. Scientific Investigations Division.. The analysis of these inorganic 11 of 18 9/19/2012 6:53 PM . The review of this material has led to a better understanding of phosphine.C. Bravenec. "Determinations of Cations in Seized Clandestine Laboratory Samples by Capillary Electrophoresis" Victor A. Chicago. Analytical data including polarimetry and derivatized gas chromatography used for the enantiomer determination is presented. "l-Methamphetamine in the Midwest" Gerald T. San Bernardino. Blaine Kern and Kerri Heward. The chemicals used are not controlled and are less hazardous than their genuine counterparts. as no testing for the gas is routinely performed. if any.[www. The results were surprising in that phosphine was encountered more often than originally suspected. USA Recipes for liquids that can imitate "liquid" PCP. DEA – North Central Laboratory. noting any social considerations which could reveal a link between stimulant abuse and each particular county (i. leading to his demise. to the possible hazards of accidental exposure. and piperidine are given. All bottles were factory labeled and factory sealed. "A Statistical and Geographic Study of Methamphetamine and Amphetamine Submissions to the Mississippi Crime Laboratory from January 1996 through June 1997" Jamela Naron Johnson.erowid.). the number of incidents where it was detected increased. DEA – Mid-Atlantic Lab. USA Many synthesis routes use inorganic components to manufacture illicit drugs. Dallas. The primary objectives of this study are: 1. and has allowed us to educate our criminalists and other field personnel. Pills from the other lot number contained no pseudoephedrine and were not visually similar. 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.. college towns. USA San Bernardino County Sheriff's seized 100 cases of Mini–Thin tablets bearing two different lot numbers. MS. more likely due to the increased awareness than by an increase in the actual number of occurrences. CA.The Clandestine Laboratory Investigating Chemists Association . Both types of pills and analytical data are displayed... etc. 2. San Bernardino County Sheriff's Department. DEA – South Central Laboratory.html Heinz body formation in red blood cells.org/archive/rhodium/chemistry/clic. Concurrent case exhibits containing other controlled as well as non-controlled substances. Mausolf. Pills from one lot number contained pseudoephedrine as expected. responding personnel are exposed. USA Seven exhibits containing l-methamphetamine were analyzed by the DEA – North Central Laboratory early in 1997. both in the field and in laboratory submissions. Diluent trends in specific areas of the State of Mississippi. Skowronski. when the presence of phosphine might be likely. CA. Inside of the room was found a discharging gas cylinder labeled "hydrogen sulfide" which was connected to tubing leading into a bucket of liquid. high incidence of motorcycle gangs. TX. To illustrate specific county distribution. Washington D. and 3. Once the odor was recognized. San Bernardino County Sheriff's Dept. Scientific Investigation Division.. 5cm effective length) x 75m I. An overview of the theory will be offered. DEA – Southwestern Laboratory. CA. CA. Observations and analysis of samples taken by the crime lab show that methamphetamine can.D.[www. sodium. DEA – Western Laboratory. magnesium. potassium. These laboratories have all been associated with a Mexican National style dump site in the Lucerne Valley which was not adequately remediated. Henderson. 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. chromium. The background electrolyte consisted of 2.7 with sodium hydroxide and triethanolamine.The Clandestine Laboratory Investigating Chemists Association . “Ion Mobility Spectrometry Demonstration” Bryan A. 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. CA. copper. reagents. USA Ion Mobility Spectrometry is a valuable tool in the detection of trace amounts of drugs. residues. liquid samples containing solids. Capillary Ion Electrophoresis (CIE) was chosen for the analysis of the cations as it provides good selectivity.. “Clandestine Laboratory Sample Characterization and Extraction Techniques” Roger A. DEA – Southwest Laboratory. CA. little sample preparation. San Diego. CONFERENCE WORKSHOPS “Carbonyl and Amine Chemistry: Continued” Harry F. Ely. short analysis time. Analysis of illicit samples of popular synthetic routes will be presented as well as detection of various cations on clandestine glassware and other containers. whereas commercially prepared HI displayed no detection of phosphate anion.html components in clandestine laboratory samples can prove to be valuable information in determining the synthesis route used. lead. "Dirt Extraction of Methamphetamine" Kerri T.25mM pyromelletic acid as the visualizing agent. Quantitation of iodide was conducted to determine the percent HI in solution with an observed linear dynamic range from 15 to 120 ppm. lithium. and thorium. precursors. San Bernardino. Scientific Investigations Division. Clandestinely prepared HI made by reacting iodine with phosphorus in water was compared to commercially prepared HI. capillary at 25°C. mercury. and equal or lower detection limits (5 to 30 ppb) when compared to ion chromatography or atomic absorption spectrometry. 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. solid organics and inorganics. This workshop will cover the examination of one. Capillary Ion Electrophoresis is a capillary electrophoresis technique optimized for the rapid determination of low molecular weight inorganic and organic ions. CA. and 0. "Anion Analysis of Hydriodic Acid by Capillary Electrophoresis" Nathan Salazar. nickel. This will include a practical demonstration of this technique in a simulation of field sampling modes. and provide tips on performing the extractions. USA Anion analysis of hydriodic acid (HI) was conducted using capillary electrophoresis (CE) with indirect photometric detection. Separation of iodide from other anions was achieved by addition of 10% methanol to the background electrolyte. Heward and Ken Lee.org/archive/rhodium/chemistry/clic. The background electrolyte was buffered at pH 7. Skinner. with 30kV applied potential.and two-phase liquids miscible and immiscible with water. in fact. These small ions lack a chromophore so Indirect Photometric Detection (IPD) is employed to obtain detection of these analytes. http://www. 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. San Bernardino County Sheriff's Department.erowid. This workshop will discuss each of the presented extraction methodologies. ammonium. smaller amount of sample (4-7hl). Analysis were carried out using a fused silica 70cm (61. strontium. calcium. San Diego. Detection of phosphate anion was observed for the clandestinely prepared HI. zinc. San Francisco. San Diego.. In this workshop. and specialized samples such as vacuum pump oils. DEA – Southwest Laboratory. be extracted from the dirt on the property in question in significant amounts. Other topics to be discussed include the 12 of 18 9/19/2012 6:53 PM .75mM hexamethonium hydroxide as an electroosmotic flow modifier. and/or solvents. The following cations are characterized: aluminum.. barium. The prosecution decided to utilize these projections in their court case. IL. DEA – Western Laboratory. forensic chemists are required to determine how much more could be made from chemical supplies present at the clandestine laboratory. processes. The presentation of often seemingly complex and technical concepts in a manner that a jury or court can understand is a challenge. The DEA agents and the local police department put questions to the laboratory as to how much methamphetamine could have been produced. adequate preparation and rehearsal allow the witness to easily convey complicated information in a simple manner.html quantitative analysis of methamphetamine and amphetamine by GC-FID.) 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 court displays cannot be understated. yet. a yield projection at this level was provided.erowid.The Clandestine Laboratory Investigating Chemists Association . “Frye vs. LC.org/archive/rhodium/chemistry/clic. resulted in the recovery of a number of full and empty pseudoephedrine tablet boxes and bottles. The use of these calculations were challenged and a Frye vs. chemist needs to perform these calculations may be based on: Primary Precursors Tablets Listed Strength Actual analysis Liquids Instrumental techniques (GC. CA. photographed. Historically. The success or failure of a forensic chemist’s testimony regarding a clandestine laboratory is directly related to the witness’s training. USA The ultimate test of the forensic drug chemist’s expertise is in the arena of the court.” The purpose of this presentation is to present several ideas on how to prepare these reports. the identification of the optical isomers of the phenylisopropylamines by derivatization using GC-FID. preparation. Cape Girardeau. USA The raid on a clandestine laboratory in Park Hills.. Semo Regional Crime Lab. The “total amount“ of controlled substance is typically calculated from the samples analyzed in the case. records (handwritten notes. Daubert hearing was conducted prior to the criminal trial. computer data. Chicago. Occasionally. “Court Room Presentations” Roger A. and reconstructions are very different from the typical controlled substance identification testimony. Missouri. etc. This approach has been affirmed by two court decisions [1. Since the sodium/ammonia reduction reaction was reported at the time to result in 90% conversion. MO.[www. In addition. etc. the values listed may be used. Daubert: How Much Meth Could A One-Armed Man Cook. These were inventoried. 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 drug made can be evaluated from this information 13 of 18 9/19/2012 6:53 PM . Testimony regarding clandestine laboratory evidence. The data that the forensic. and some tips for improving phenethylamine chromatography. and released to the hazardous material disposal unit. DEA – North Central Laboratory.. the production capability has always been calculated as the amount of controlled substance that could be manufactured at the 100% theoretical yield.2]. “Production Capacity Reports” Gerald Skrowonski. If A One-Armed Man Could Cook” Pamela Johnson.. but may also be called upon by prosecutors to prepare a “Production Capacity Report. Ely. USA A forensic chemist may not only have to analyze evidentiary samples from a clandestine laboratory. This workshop will provide some suggestions and salient points to consider for the clandestine laboratory expert witness. San Francisco. experience and breadth of knowledge. http://www.) are found at clandestine lab sites indicating past drug production. CO. The future of case law in this area will be discussed and the successes and failures in the legislative arena.A.. Aurora Police Department. 1. especially in the pharmaceutical industry.. 4. 14 of 18 9/19/2012 6:53 PM . 2. 1997 search warrants were served at two locations southwest of Indianapolis. and finally.html and. “Protecting Group Chemistry” Tim McKibben. 1383 (8th Cir. SmithKline Beecham Pharmaceuticals. Animal and botanical sources of tryptamines and related analogs. TX. Eight individuals. which can then be subjected to reaction conditions. 3. These “protected“ intermediates or precursors have been encountered by forensic chemists and should be familiar to chemists investigating illicit drug manufacturing cases. The pharmacology of tryptamine derivatives in terms of structure activity relationships. CA. King of Prussia.org/archive/rhodium/chemistry/clic. Wagner. but. One of the individuals arrested was charged with the manufacture of methamphetamine. Both of these issues will be discussed. It will also be shown why child endangerment is not a viable theory for criminal liability in a murder trial. USA Protecting group chemistry involves the use of reagents to convert a functional group into a “protected” functional group. which would otherwise destroy the unprotected form. El Paso. This presentation will introduce the forensic chemist to some common protection groups and techniques used to add and remove them from the chemical intermediate. 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. “Tryptamines and TIHKAL” Andrew C. if pertinent. 96 F.D. This technique is commonly used throughout organic chemistry.. Lawrence. Finally. Ph. Riverside. be based on the total amount of “Mexican Drug Trafficking Situation Brief” Robert N. PA. were arrested. The location of his lab and the synthesis routes used were unusual.D. Davis. USA On February 13. therefore any calculation must methamphetamine that the defendant was in a position to produce). United State v. 6. Current methodology being utilized by these organizations will be detailed. Indiana State Police. Allen. USA An overview of drug-trafficking organizations operating in Mexico and the United States. “The Kathey James Story” D. Evans and Thomas J. DEA – EPIC – Operational Intelligence Unit. The synthesis of indole and substituted indoles. was novel in his approach to the manufacture of methamphetamine. United States v.[www. Riverside County District Attorney. along with a historical perspective of the Mexican Drug Trafficking Organization. 1992) (The defendant's purpose here was to manufacture methamphetamine. 1989) (Maximum amount of methamphetamine that defendant could produce was used in determining base offense level even though defendant inexperienced). At the end of this presentation — a taped interview with the “cook” explaining how he made the dope will be viewed.S. Harding.2d 1090 (8th Cir. IN. 2. as well as the relationship to criminal organizations operating along the U./Mexico border. Examples of protection group chemistry used in illicit and legal manufacturing will be presented. Commercial sources of indole analogs as precursors to tryptamine analogs. 884 F. What makes this case unusual is not only that the “cook” was employed by a large pharmaceutical company. 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.. while a reasonable percent yield for the particular synthesis employed in the clandestine laboratory is not included in the capacity report. part of a distribution ring dealing in methamphetamine.2d 1380. Indianapolis. 5. “A Cookers Dream” Eric L. Beshore.The Clandestine Laboratory Investigating Chemists Association . The topics of discussion will include: 1. be included in the report. Personalities will be identified. http://www. Aurora. John M. The synthesis of DMT and related analogs. USA Tryptamines and their significance to forensic science are the subject of this presentation. Shamanism and its historic role in the use of these hallucinogenics.erowid. The garage. and 235 gm of DMT. 200 S Lena Rd. leading to his demise. the open valve on which he was unable to close. Criminalist. consistent with the final step of methamphetamine manufacture in which the drug is salted out using hydrogen chloride gas. Forensic Specialist Rice also assisted in photographing the exterior of the scene.erowid. Near the body of the deceased was a half-face air purifying respirator (APR) equipped with organic vapor cartridges. Laing. Supervising Criminalist Hiram Evans and Forensic Specialist Karen Rice assisted the Deputy Coroner with an examination of the body of the deceased. they were directed by Sheriff's Narcotics Detectives to the body of a deceased Hispanic male in his late twenties. 15 of 18 9/19/2012 6:53 PM . and DMT in a clandestine lab setting? Answer: Conspiracy. enter the key figure of Nicholas Sand.00. fire department and Coroner's representatives. Anjaria. MDA. following a lengthy investigation. Criminalists Mehul B. the records indicated gross wholesale sales in excess of $1. CA. Criminalists Anjaria and Kern processed the interior of the garage. After conferral between the various law enforcement. converted to living quarters. international distribution networks.html “A Career ‘High’” Richard R. MDMA. and multimillion-dollar production capacity. These sales represented the distribution of 127 gm of LSD..[www. indicating that the cylinder was freely discharging. sophisticated laboratory setup. 500 gm of MDA. lying supine on the driveway adjacent to what had been the garage. Evans. 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. Canada Question: What do you have when you seize large quantities of LSD. Scientific Investigations Division. notes. HYDROGEN SULFIDE FATALITY Mehul B. The seized chemicals. Health Canada. 4800 gm of MDMA. TEXT On January 30. hydriodic acid.The Clandestine Laboratory Investigating Chemists Association . San Bernardino. 1997.866. http://www. noting a gas cylinder labeled “hydrogen sulfide” with ice formed on the bottom potion of the cylinder. The wallet contained some peso notes and a California Driver's License (CDL). including rolling set of inked fingerprints and recovery of his wallet. 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. Hiram K.000. convicted in absentia for the manufacture of LSD. He had been a fugitive for over 20 years. located to the rear of the residence. and other items commonly associated with the clandestine manufacture of methamphetamine. “COOK” FAILS CHEM 101. In the year proceeding the seizure.. Burnaby. On arrival. The cylinder was connected via tubing to a 5 gallon bucket containing liquid. and ledger sheets all depict a large commercial manufacture and distribution operation. Also present in the building were two-phase liquids. BC. a mop bucket equipped with a press. although the CDL photograph did not particularly resemble the victim. All of these were found in a Vancouver suburban clandestine laboratory that was seized September 26. Due to the hazardous nature of the environment. additional air cylinder for the SCBAs were requested. multiple identities. Anjaria and Blaine M. Kern responded to a suspected clandestine drug laboratory in the Muscoy area of San Bernardino. Criminalists Anjaria and Kern donned protective clothing and SCBAs and entered the converted garage. it was decided to move the body of the deceased upwind from his original position to facilitate the examination of the body. To add intrigue to this case. 1996. red phosphorus. Supervising Criminalist/Deputy Sheriff San Bernardino County Sheriff's Department..org/archive/rhodium/chemistry/clic. lye. . Whether the “cook” obtained it on his own or through others is unknown at this time. Vapor concentrations as low as 50 ppm in air cause toxic symptoms. Reportedly. 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. 147.The Clandestine Laboratory Investigating Chemists Association . Small disposable glassware. CA 93710-5856 AT CALIFORNIA With increasing frequency. p. is employed to contain the ingredients. By the way of comparison. heavier than air.org/archive/rhodium/chemistry/clic. With the sense of smell fatigued. No red phosphorous is used. 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]. flammable gas having the characteristic.. but kills through respiratory paralysis [2].. 1957. Dangerous Properties of Industrial Materials. but in contrast is lighter than air. flammable gas. Willaims & Wilkins Co. 888.erowid. 12th ed. 300 ppm is immediately dangerous to life and health (IDLH). those exposed fail to get warning of high concentrations. 16 of 18 9/19/2012 6:53 PM . it is an insidious irritant and chemical asphyxiant which fatigues the sense of smell.. This 3 2 large scale reaction using H O P is unusual. Irving Sax. N. One chemist reported that a 12 liter round bottom flask contained a reaction mixture which utilized H O P. Baltimore.” While the odor of hydrogen sulfide is detectable at very low concentrations.. pungent odor of 2 rotten eggs. Marion N. Page.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. The acid is simply poured onto the starting material and iodine crystals. with a 50 ppm IDLH level. Merck Index. 1996. but not the name given on the CDL. 3. Gleason. Rahway.[www. as a reaction ingredient at clandestine methamphetamine laboratory scenes. In 3 2 August 1996. Fresno. organic vapor. Efficiency of the reaction procedure is unclear and has not been established from field observations. 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%. http://www. 1963. as little as fifteen minutes of heat has been applied. Hydrogen sulfide (H S) is a colorless. and Harold N. Co.. hydrogen cyanide (HCN) is also a colorless. 2nd ed. REFERENCES 1.. Clinical Toxicology of Commerical Products.. NY. HYPOPHOSPHOROUS ACID USE INCREASES CLANDESTINE METHAMPHETAMINE LABS Jerry Massetti. ed. Bullard. California crime lab personnel who process clandestine lab scenes are recognizing hypophosphorous acid. Criminalist CA DOJ Crime Lab. MD. w/w). Acid gas. 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. and 1000-2000 ppm is usually fatal within minutes [1]. p. 823. Robert E. New York. Since then it has become apparent that H O P is being used 3 2 in most parts of California. p. 2. having a characteristic faint odor. 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. 1704 E. Susan Budavari. such as a canning jar or a beer bottle. H O P. NJ. Gosselin. and base cartridges generally utilized in APRs are marked to be used with hydrogen sulfide “for escape only. leading to respiratory paralysis and sudden collapse [3]. Reinhold Pub. 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. contact: Steven B.10. J. Clandestine Laboratory Investigating Chemists Association. No 2.. 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. For more information regarding the monographs or to place an order. 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. Clandestine Laboratory Investigating Chemists Association. but did not consider it as a reaction ingredient and did not sample it at the time. 6. 5. The compiler(s) of the monographs present the monograph at the meeting and discuss the organization and content. One half liter of 50% 3 2 H O P can be obtained for as little as $14.[www. Methamphetamine lab scenes using H O P have been very common in Australia for a number of years. http://www. the amount of H O P reported to this program has more than tripled from $18. Others have indicated that they were not aware of its usefulness for manufacturing methamphetamine. p. Johnson Los Angeles PD Crime Lab 555 Ramirez St Ste 270 Los Angeles. an informal poll of many crime labs 3 2 in California was made. 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). At the seminar. In about a two year period ending December 1996. Vol.org/archive/rhodium/chemistry/clic. J. October 1996. pp. No 4. A 1-gallon sized bottle of H O P was 3 2 found at a clandestine methamphetamine lab fire scene. Vol. Another reported that an unlabeled acidic solution containing phosphorus was retrieved from a scene.844 to $60.383. Johnson reported containers of "Plating Solution" to contain a mixture of acids consisting mostly of hydriodic acid [2]. DRUG MONOGRAPH AND REFERENCE MANUALS The Association presents a new drug monograph series each year at its Technical Training Seminar. 13.Fax Drug Monograph and Reference Titles Shipping cost Price (per set) US Foreign 17 of 18 9/19/2012 6:53 PM . CA 90012-6302 (213) 237-0041 . A number of chemists have stated that they actually have observed H O P at 3 2 meth lab scenes.. January 1992. April 1995. 3 2 Vallely described its use as a reactant [3]. 2. 10. J. In 1995. Others indicate that it would not be identified in their analytical procedures. Skinner discussed the reducing capacity of H O P at the 3rd Annual CLIC 3 2 Seminar at Memphis (1993). 14-15. Most chemists / criminalists have not encountered or recognized H O P at a 3 2 methamphetamine lab investigation. 2.erowid. No 1. Vol. Clandestine Laboratory Investigating Chemists Association.html Chemical cash sales reported to the California Bureau of Narcotics Enforcement / Clandestine Lab Enforcement Program (BNE / CLEP) corroborate lab scene observations. 1.Voice (213) 237-0040 . 3. Please note the manuals are only shipped to forensic laboratories throughout the world on a confirmation basis.The Clandestine Laboratory Investigating Chemists Association . Subsequent to Kern County’s report of H O P’s use as a reactant last August. but was not characterized further. p. Cash sales of chemicals in California exceeding one hundred dollars are required to be reported to BNE/CLEP. In January 1992.. A listing of the current monographs and references can be found below. the monograph is provided to the attendee as part of their registration packet. The Association is pleased to offer these monographs and references to other forensic drug chemists for sale. 1994 A Review of the Synthesis and Analysis of Phencyclidine and Its Analogs (1 volume). Allen. compiled by M.. 1993 Structure-Activity Relationships.00 $10.50 $2. Synthesis. compiled by A. compiled by K. Yeung. Weaver and E.The Clandestine Laboratory Investigating Chemists Association .A.A. http://www..50 $7.F. Dal Cason. 1996 18 of 18 9/19/2012 6:53 PM . Amphetamine. Kalchik.00 $65. Kalchik and R.50 $7.erowid. compiled by M.50 $7.org/archive/rhodium/chemistry/clic. 1995 $35.00 $15.F. and Methamphetamine(2 volumes).50 $2. 1995 A Review of the Synthesis and Analysis of Fentanyl and Its Analogs $15.00 $5.00 (1 volume). Precursor Preparation and Analysis of Methylenedioxyamphetamine and Its Analogs and Homologs(4 volumes).html A Review of the Synthesis and Analysis of Phenyl-2-propanone.. compiled by T.C.00 (1 volume).50 An Analyst’s Guide to the Investigation of Clandestine Laboratories $15. Ely.00 $10.00 $15.[www.00 $2.
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