the construction and operation of clandestine drug laboratories - j b nimble, loompanics 1994

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    The Construction And Operation of Clandestine Drug Laboratories 1

    Editor & Transcribers Introduction.

    This is not an exact copy of the original. Somespellings have been corrected & changed to theBritish. Many sentences have been completelychanged (with the meaning staying the same).

    Some bits may even have been added. 95% ofthe original book is still here.

    Experimenters should also check out articlesfrom old Scientific American about home-madeapparatus (there is a CD compilation of themavailable) and the J ournal of Chemical Educationhas many excellent articles on money savingdevices for chemistry.

    Always use borosilicate glassware or plasticcontainers if you are using heat, soda-glass isntworth the risk. Beware of using glass-ware with

    flaws in it (youre likely to get some of these ifyou buy second-hand). Get the ChemicalTechnicians Ready Reference Handbook byShugar & Ballinger [Pub. McGraw Hill] and/orThe Laboratory Companion, by Coyne [Pub.Wiley.]. Go to college and study chemistry.

    It goes without saying that this book is well out-of-date.

    The Construction And Operation ofClandestine Drug Laboratories

    Second Edition,1994 by Jack B. Nimble

    This book is sold for information purposes only.Neither the author nor the publisher will be heldaccountable for the use or misuse of theinformation contained in this book.

    All Companies and other commercial entitiesmentioned in this book are casual observations offirms that appear to produce quality equipmentsuited to an industrial type environment, period.Positively no statements or implications are giventhat any of these entities Produce or sell productsintended for any illegal or unethical use.

    All rights reserved. No part of this book may bereproduced or stored in any form whatsoeverwithout the prior written consent of the publisher.Reviews may quote brief passages without thewritten consent of the publisher as long as propercredit is given.

    Published by:

    Loompanics UnlimitedPO Box 1197Port Townsend, WA 98368

    Loompanics Unlimited is a division ofLoompanics Enterprises, Inc.

    ISBN 1-55950-108-1

    Library of Congress Card Catalog 93-80258

    Cover by Daniel Wend/MEDIA Graphics

    Illustrations by J ack B. Nimble

    Contents

    Preface to The Second Edition 1The Risks 7Security 13Scanners and Monitoring Equipment 23Safety 27Location and Facilities 31When to Stop and How 35Glassware 37Heating, Stirring, and MixingFume Hoods 57Miscellaneous Equipment 67Scaling Up 77

    Procurement of Suspicious Items 85Tablets, Capsules, and Other PackagingMaterials 99Computers 107Appendix 1: More Equipment 111Appendix 2: Watched Chemicals 113Appendix 3: Watched Laboratory Equipment 115Appendix 4: Legitimate Businesses that use

    Laboratory Equipment 117Appendix 5: Common Products and the

    Valuable Chemicals theyContain 119

    Appendix 6: Recommended Reading 121

    Preface to the Second Edition

    Well, the 1990s are now with us and much haschanged since the first edition. The War onDrugs, increasing cooperation of chemicalsuppliers, product liability-awareness, andstringent new regulations have made operating aclandestine laboratory more challenging (andprofitable) than ever.

    Sadly, we now live in a world where lawsuits andlobbying legislate regulations and dictate

    behaviour in the business world. This book is soldfor informational purposes only. The informationcontained herein is my opinion. I do notencourage anyone to break any law, or violateany local, state, federal, or international statutes,guidelines, regulations, building codes, zoningordinances, or anything bearing a remotesimilarity. If you are unsure of the legality ofanything you do, or think of doing, or are about tothink about doing, I urge you to seek out theauthorities and question them!

    Please understand this book concerns building

    and operating a laboratory - it is NOT a book ondrug chemistry. Don't ask me how to synthesisethings. There ate already many good books

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    The Construction And Operation of Clandestine Drug Laboratories 2

    available in that arena. Michael Valentine Smith'sPsychedelic Chemistry is one of particular merit.It could use a better index, but it's still excellent.All procedures include scientific literaturereferences, so you can dig up the originalpublication. For the phenethylamine

    (amphetamine) class of drugs, Dr. AlexanderShulgin's Pihkal is "the book." His philosophy ondrugs is illuminating too. I am also grateful to themany persons who have shown me theirlaboratories in recent years - their ingenuity andmistakes are fully reflected in this edition. If I canbe allowed to generalise, these labs seem todivide into two distinct categories. One, you justwant to hurry up and get the hell out of beforesomething blows up, or the police dynamite thedoor. The other kind, you just have a deep downfeeling that everything is cool. There are no nastysmells, the property fits in with its surroundings,

    there isn't powder dried all over the counter top,scores of tin cans everywhere with remnants of"bad batches," or empty chemical containers inthe trash with the labels still on them. Whichcategory do you fall into?

    I've been criticised on occasion for not presentingthe reader with enough specifics. I would like torespond to this. My attempt in this book is tointroduce the reader to various ways aclandestine laboratory is built and operated, witha variety of materials and situations. I haveincluded specific examples of how these methodshave worked well for myself and others. If you are

    a person who must have a specific diagram infront of you, listing every part and its exactspecifications, as well as instructions that tellinstructions that tell you exactly where to buyglass jars and plastic spatulas - you'll probably bedissatisfied with this book. I would be surprised ifyou ever actually operate a successfulclandestine laboratory. I would also guess thatyou were probably looking for a book that you canpick up and read that will make you an expertchemist. This hobby requires that you beresourceful. You should have things like achemical compatibility chart on your wall forreference; and, you should be able to recognisethe differences between polycarbonate,polyethylene, Teflon, etc. Such knowledge meansyou don't dissolve that kitchen cup you're about topour your solution into. I've included many moresources of information in this edition.

    Like anything else, you will only become good atchemistry through experience. A degree inchemistry will certainly give you a flying start, butyou must learn most of it through experience.Most drug manufacturing procedures fall underthe category of "organic chemistry. This means

    simply the chemistry related to carboncompounds. Organic chemistry is a very seat-of-the-pants type of science. Most of the learning

    takes place in the laboratory, not on achalkboard. I have many times duplicated apublished procedure exactly as described -downto the identical equipment, identical quantities,and same sources of the reagent chemicals -nearly always to find a significant difference in

    yields, temperatures, reaction times, etc. It is onlythrough experience that you learn to steer astraight path through these perplexing momentswith a solid feeling for what is correct procedure.

    And let me take a brief moment to interjectsomething that you will probably be surprised tofind in an underground-drug publication: adiscussion of ethical behaviour. You will of coursedo what you want to do, but let me enlighten youjust a tiny bit about "responsibilities."

    All drugs are not created equal. You must alwaysremember that your fellow humans are trusting

    you greatly (sometimes ignorantly) when theyingest your creations. It's easy to look at thatsemi-pure powder and convince yourself it's goodenough, and forgo the final rinse orrecrystallization. Don't be the brown-powder foolwho proclaims: "Hell, man, it never made mesick..." Many people are hypersensitive to the by-products you neglect to remove from your batch.Of course, you have no control over the quantitypeople will take, if they will abuse it excessively,have a bad trip, freak out, etc. If youmanufactured motorcycles, people would buythem and drive like marauders, and, eventually,

    someone would get hurt on a machine you made.Perhaps it was their recklessness, or perhaps itwas that axle nut your assembler forgot totighten. Perhaps you manufacture kitchenknives? Eventually, someone will cut themselves,even use one of them to commit suicide ormurder. My point is: you simply have to do thevery best that you can do, and always rememberthat others (many you will never meet) aretrusting you greatly. You owe it to all concernedto always deliver consistent purity and dosages.

    One final word on this subject: your choice ofproduct. Exactly what are you making?Personally, I would have a big problemmanufacturing crack, ice, methyl-fentanyl, etc., formass distribution and consumption. These are aspecial breed of drugs that seem to perpetuallytorment the user and imprison the dealer. Leavethese substances to the fools dumb enough tomake them. It is my sincere hope that theinformation I present here is used with goodintent. Clandestine chemistry can be grosslyprofitable. It is unfortunate that good ideals areoften lost in the midst of huge profits. This book isfor those wonderful people who value freedomand the human spirit above money and power.Perhaps if these people begin to voice theiropinions mote, the day of responsible drug use,

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    The Construction And Operation of Clandestine Drug Laboratories 3

    manufacture, and control will become a reality.Enough said.

    Manufacturing drugs can involve a certain degreeof risk, which varies from country to country.Unfortunately, I have had several acquaintanceswho have lived through the nightmare of a bust.

    In this second edition, I share some of their "whyand how" stories with you.

    This edition also seems to breathe a more militanttone than the first. This is not really intentional. Itis simply a reflection of the environmentsurrounding clandestine labs at this time. TheWar On Drugs, Inc. has become an entireindustry, sucking up billions of dollars and feedingitself with lots of high profile media coverage.Drugs are blamed for everything: poverty, crime,AIDS, even threats to national security. Everyonehas seen the crack-house busts on TV, with

    police agents decked out in full tactical gear andarmed with automatic weapons. You've seenthem storming into private homes, often withsmall children inside. They seem to never showone of the 45 percent that end up in no arrests.And you hear them proclaiming loudly that they'rewinning this "war!" The entire criminal legalsystem is clogged daily with thousands of minordrug possession charges. J udges are oftenhanding out 20 years to life for drugs while rapeand violent cases settle for less than 5. Even adeath penalty for drug "kingpins" has beenproposed.

    Well, I doubt seriously if things will changeanytime soon. I have stopped spending so muchtime worrying about when the Drug War will bedeclared a truce, and I have omitted much of mybitter treatise on drug politics from the firstedition.

    I am not suggesting I have the answer to drugabuse. I wish only to illustrate how the presentsystem consumes valuable resources andworsens the problem, in spite of a few goodintentions.

    The clandestine laboratories described in thisbook don't have to be used to make illegal drugs.They could be used to manufacture medicinesand useful chemicals in war or survival situations.This book contains what I know about setting upand operating clandestine laboratories. It is soldfor informational purposes only. The Risks

    The Risks

    Throughout this book I put great emphasis on theDEA, and less on local enforcement agencies.Why? If you're a careful, proficient chemist, youprobably won't get busted... the odds are tipped

    in your favour. But if you do, even though you'recareful and proficient, it will probably be from alead developed through your chemical (or lab

    equipment) suppliers, which generally cooperatewith the DEA rather than local units. If you are asloppy crank lab, your neighbours will think youlook suspicious and call the local police. They'llcome out, go through your trash looking for clues,probably find some, probably smell your lab, and

    even go in on probable cause. If you are bustedas a result of a larger investigation working itsway backwards from some street dealer whoplea-bargained, it could be the DEA, or perhaps alocal task force. Most communities have thesetask forces, (which are part of the local policenetwork), set up for the specific purpose ofperforming drug-related raids. Many of them aretrained and equipped like the Green Berets orSpecial Forces. They enter premises withbattering rams that will break solid concrete,shoot tear-gas and noise makers in through thewindows, and use automatic weapons. If you find

    yourself vying to "prepare" yourself for anencounter with these guys, then I seriouslyquestion your sanity and intelligence. Not beingdiscovered in the fist place is the only sensibleplace to put Your efforts.

    Never underestimate forensic science when youthink you're disposing of evidence. Fingerprints,traces of saliva, hair, skin cells, foot prints, nearlyanything you deal with can be traced back to you.There is no way to eliminate all the holes. Themost important thing is not getting discovered inthe fist place. Keep traces of drugs off the thingsyou throw in the trash, or anything else that will

    be accessible to other people (even envelopesand paper!). There are cases on the books whereagents scraped the residue of a drugintermediate (even precursors) out of containersthat chemists have left outside or thrown away.This evidence easily leads to probable cause.

    Most drug users, dealers, and manufacturers aresent to state penitentiaries. In a few cases, suchas federal tax evasion, money laundering, federalanalog laws, and similar federal raps you may goto a federal prison. These are a bit better, as ageneral rule. But don't count on it just because

    you're manufacturing some exotic analog. You'llprobably still spend time in a hell-hole statefacility.

    Fortunately, as of this writing, the justice systemis being forced to release non-violent/non-repeatoffenders to make room in crowded prisons. Thisis just one more reason not to have lots of gunsand ammo laying around in your lab.

    Prison is a horrible environment to spend your lifein. It's even a horrible place to visit someone youknow. Fortunately, I have never spent a singlenight in a jail cell, but I've talked with and visited

    many who have, a couple of them very goodfriends. I will share a few of their stories with you.

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    The Construction And Operation of Clandestine Drug Laboratories 5

    Security

    One of the finest skills to master is silence.Unconditional silence. Mistakes made here willcost you time in the slammer, maybe even yourlife. I cannot stress enough how importantanonymity is.

    I have backed off a bit from my stance in the firstedition that anything but a one-person operationis insane. That's unrealistic. At some point oranother you will have to deal with someone elsein the course of business. J ust use thesereminders as guidelines: Few chemicalprocedures require more than two hands.Working alone means no one to snitch on youlater. It also means no one to argue profits andoperations with, and no one to seam some of theharvest while you're not watching. Few chemists,if any, are caught who truly act alone. The many

    voices of experience echo: "work alone." Butworking with someone is fun, and it makes forgreat conversation and stories a few years laterwhen you're sitting around having a beer:

    "...that time when we dumped that 55 gallonbatch down the drain thinking it was waste... andthat time we improvised the outboard motor for anemergency stirrer.. and that time the landlordwalked in the back door, and that time we... "

    Security also means unobtrusive behaviour onyour part. Cover all your tracks. Have good rusesready for any nosy person. If a neighbour

    complains about an odor, say you spilt somecarburettor cleaner or plating bath or somethingelse like that. Act as if the smells are equallynoxious to yourself, say "sorry," and shut downcompletely for a while. Never leave glassware,empty chemical containers, chemistry books, orlab equipment in sight of others. Do not ever havechemicals or lab equipment sent to yourresidence or place of manufacture. Postal andDOT regulations require conspicuous warninglabels on many chemical shipments. Packagesare often left with neighbours if you're not home.Also, never leave these empty shipping

    containers out on the curb or alley to be taken offas trash. Tear off all labels, put them in opaquetrash bags and throw them in a dumpster acrosstown.

    Always completely eliminate visibility into yourworking area. Police now routinely use videocameras and night-vision scopes to obtain searchwarrant evidence. Frosted glass is good, andallows light to enter. The spray-on glass frostinghas a tendency to flake oh. A white curtain letslight in, and blocks the view even if the window isbroken. Aluminium foil is overkill and looks

    suspicious. I've seen some people put up acurtain then fasten a flat black piece of plywoodbehind that. From the outside, it looks like a

    normal room with the lights off all the time. It alsoprovides protection against anyone enteringthrough the window.

    Perform smelly distillations and evaporationsduring late hours when most people are asleep,and do them under a fume hood. Foul weather is

    another good time as few persons will be outside.Rain also has the remarkable ability to cleansethe air of odours. The chapter on fume hoodsdiscusses the elimination of odours in detail.Beware when working with ether. Its strong anddistinctive odor has blown the cover of manyclandestine labs. It's also extremely flammable.Use an alternate solvent unless you have theproper equipment and facilities. Ether is a smelly,dangerous solvent. I discuss ether in more detailin a later chapter.

    Keep drugs out of your laboratory. Store them in

    a secure, obscure, and confidential place aftermanufacture. Thoroughly wash all glassware andequipment with a good detergent. Follow with anacetone (or similar) rinse afterwards. Your taxdollars have purchased elaborate, expensiveequipment that forensic narcs use to detectmolecular-sized traces of most drugs. Don't everunderestimate the prowess of forensic chemists!The World Trade Centre bombing in 1993 was agood example of how much information is buriedin residual evidence, even after an explosion.People who tell you that setting your lab on fire(to destroy evidence) when you hear the doors

    being kicked in are not informed. You'll only addan arson charge to your legal troubles.

    Watch spills - clean them up thoroughly. Don'tleave drugs in various stages of production layingaround to be completed "later." Finish up, clean-up, and get the stuff out of your laboratory. Beable to pack up your entire operation (chemicalsand fancy equipment, that is) on a moment'snotice. Have with you at any given time only thechemicals and equipment you need for a givenprocedure.

    Know where the toilet is, and be prepared to

    dispose of as much contraband as possible on asecond's warning. Even though you may stillhave evidence around, you'll be much better off incourt with 0.23 grams than with 2 pounds.

    Watch for surveillance too. Physical surveillanceis not hard to spot if you continuously look for it.Cats, vans, and recreational vehicles arenotorious as tools of surveillance used by narcs.Wire taps and pen registers are common as well.Never discuss any aspect of drugs on yourtelephone. Avoid suspicious innuendoes andlingo too. Should you suspect surveillance, stop

    then. Cease operation for several months.Surveillance is very expensive. It involves a lot oftime from highly paid persons. Even pen registers

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    The Construction And Operation of Clandestine Drug Laboratories 6

    (a listing of all numbers dialled on a particularphone) require much time and money to analyze.For these reasons, surveillance is usually ceasedif positive evidence is not being produced. Beirregular. Never make promises about exactdelivery times, sales, etc. Maintain the ability to

    stop at any time. The added margin of security iswell worth any inconveniences from an irregularschedule. Think ahead and you won't be sorrylater - and always consider very carefully takingon a partner.

    What are the communication requirements of theclandestine chemist, and how can they be safelysatisfied? Later I will discuss the use of ananswering service. Never give a chemicalcompany your home telephone number, or anyother number that can be traced directly to you.Finding to whom a particular telephone numberbelongs is a simple phone call for any local, state,

    or federal official. You must also be very selectiveabout whom you place calls to from your phone,as this information (the actual numbers that youdial) is also readily available without a warrant.Caller-ID is available in many areas, displayingyour number on someone's phone before theyeven answer it! This is where a handful ofquarters and a payphone with some privacy areimportant. Be sure to prepay more time than youever expect to use. It would be awful to have arecording say, "You have one minute left, pleasedeposit 75 cents for three additional minutes,"just as you were closing that deal on 20 lbs. of a

    hard to get precursor.

    Few persons know exactly how many wiretapsare made each year, and while I personallysuspect the number is small, you should alwaysassume that everything you say on the telephoneis being monitored. The consequences of anunknown phone tap are usually devastating. Andwhat about cellular phones? While they mayprovide a degree of ambiguity regarding the exactorigin of a call, they are more easily monitored,and present fewer legal obstacles for theauthorities to intercept. In fact, there is an entire

    hobby developing in this country of monitoringcellular and portable phones. More than once, thepolice have got solid leads and developed usableevidence based on the numbers stored inconfiscated cellular phones (and pagers). Nearlyall cellular phones remember the last number youdialled so you can use a "redial" button. Also, anew technology known as "cellular mapping" hasrecently become available that allows the locationof a cellular phone to be generalised, even themovement from "cell" to "cell" as a moving callerprogresses. The most disturbing thing of all is thatthey can apply this type of "trace" to calls made

    months (even years!) ago, using the informationthe telephone company can provide. The bottomline? Try to use telephones of any type (and

    pagers) as little as possible. When you must usethem, use pay telephones.

    Drug laboratories are busted all the time. Thetypical scenario is a speed lab in a garage withdozens of jars laying around, no exhaust fan,empty drums in the alley, souped-up cars in the

    driveway, etc. Watch the news and you can learnfrom others' mistakes.

    Often, busts occur because of the lab's audacity,not from a police investigation. I was watching thenews recently, and a laboratory in Los Angeleswas busted when neighbours noticed noxiousyellow smoke seeping out from under the garagedoor. The fire department was called, and theywere inside the garage before the resident evenknew they were there. Inside was really a mess:loose exposed wires, clutter all over the floor anddozens of half-full chemical jars. If you have a fire

    or other disaster, it is usually legal for emergencycrews to enter by force, and any evidence foundis considered obtained in "good faith." Keepeverything neat and clean. Believe me, I tried it alldifferent ways, and neatness always works best.You'll make more product, you'll be under lessstress while you work, and you'll sleep better atnight.

    Similar circumstances arise if your place isburglarised or vandalised. This problem iscompounded if you have a monitored alarm thatgoes off. I would stay away from alarms. The bestinsurance is to keep the lab hidden even from aburglar that's already inside. A heavy door andlock are a must. My favourite dead-bolt is thenearly pick-and-drill-proof Medico. Combined witha steel door they provide a very securepassageway. Don't forget windows either.Frosted glass is great, but suppose someonethrows a rock through the window? Is your labstill out of view or is a giant peephole now visiblefrom across the street, right into your workspace?

    Out in the country, a large dog (or two) are greatfor keeping people away from your operation. Noone is likely to smell anything if they can never

    get closer than 500 yards to your lab. In the city,they are great to have inside while you are gone,to prevent burglary. Even the most desperatesoul will not likely enter the premises should theyhear barking inside. My personal favourite labdog is the Rottweiler. Their appearance is veryintimidating, they become very attached to their"pack" (you), and they seem to naturally developa "protect and serve" disposition. Like no otherbreed, they can smell out trouble. Females areespecially loyal. For a lab dog, seek one that islaid-back and not hyper. Treat your dog well, andnever ever let them "sample the batch." Dogs are

    much more sensitive to many drugs thanhumans, and probably wouldn't enjoy it anyway.Besides, you want them on their toes to listen for

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    The Construction And Operation of Clandestine Drug Laboratories 7

    intruders. They're also great company, help calmyour nerves, don't rat on you later, and don'treally care if what you're doing is legal or not. Irecommend dogs.

    Safety and security are tightly related. Take alook around and ask yourself, "What is the worst

    disaster that could happen here?" And then ask,"Could it contain itself?" Ideally, your lab has ahigh ceiling, concrete or brick walls and a cementfloor with a drain. Kept clean, this environmentwill handle all but the biggest mishaps withouttaking your house with it. One fairly new productto hit the market in recent years are the self-contained Halon fire extinguishers. These unitsmount against the ceiling, or inside a cabinet.They are equipped with a fuse that melts at 160degrees F. They then flood the area with Halongas, which quickly quenches nearly any type offire and leaves no residue - so you might even

    salvage your batch. Afterwards, they're refillable.Make sure you get one for the proper size areayou wish to protect (their capacity is rated in cubicfeet), and remember they only work best inenclosed places. So keep one or two inside yourfume hood, another inside your flammablesolvents cabinet, etc. They are cheap insurance.At least consider a large manually operatedHalon extinguisher.

    Anyone who has experienced a clandestinelaboratory fire knows what an absolutely terrifyingexperience it is. It usually happens very suddenly,

    and as you struggle frantically to get it undercontrol your mind is racing through manythoughts. Is it bad enough to call the firedepartment? Should I try to destroy as muchevidence as I can first? What can I tell them thisplace is? Should I just get out now while I can,and before my solvent cabinet explodes? Theentire scenario runs its course in minutes, evenseconds - your life and freedom are put right onthe line. You might die, you might go to jail, youmight lose your lab and all possessions, or youmight put it out, continue your synthesis and bejust fine. I have experienced one fire, and that

    wised me up quickly. I vowed never to put myselfthrough that trauma again. A teal grey-hairgrower.

    Also on the subject of security, I have includedthe details of an engineering marvel. This deviceis a kick-in proof, battering-ram proof door that anenterprising gentleman has constructed. This sonof rubbed me the wrong way at first, as I thinkefforts should go into not being discovered in thefirst place. But I was so impressed with thisdevice I just have to share it with you.

    From the outside, this door looks rather

    innocuous. But the secret lies on the other side. Itstill requires a firmly seated jamb, so I wouldn'trecommend it in a wood frame house. The lamb

    (frame) of this door is fitted with many automobilevalve springs that absorb the impact of any blowsand return it instantly to its original position.

    This entryway looks like anordinary commercial steel dooron the outside.

    It is especially easy to constructusing a "pre-hung' steel doorand jamb.

    A Metal brackets are bolted into wallwith long masonry bolts.

    B 11-15 springs are a good number

    Adding more makes the mechanismtoo stiff and forces the door to absorbmore energy.

    C Strips of 1"x1" x" angle steelgreatly reinforce the door itself.

    D The door jamb is "floating - it is held inplace only by the great force of thevalve springs.The stops in front of the door limit itsforward travel.

    This one was constructed with a rather thin (inch) piece of steel as a cover for an ordinary

    wood door. Angle iron was used to reinforce itfrom the back. We tested it, and the door won.Using a 3 inch pipe 5 feet long and filled withcement, we rammed and rammed until we couldram no more! We marred the surface of his doorup quite a bit, though no structural damageoccurred whatsoever.

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    A door like this could buy you some precious timeto dispose of contraband until they figuredanother way into your place. This door is the only

    thing like it I've ever seen. People who justreinforce a door with steel often find out that abattering ram will punch the whole door rightthrough a brick wall - there's nothing to absorbthe energy. I'm sure many improvements couldbe made to the design of this door. This samegentleman was already working on a "cutting-torch proof" door! If he's successful, and I eversee him again, I'll share his ingenuity with youagain in a future edition.

    Scanners and Monitoring Equipment

    I've been monitoring the DEA's communicationsfor nearly seven years now. (In fact, I am listeningto them as I write this!) And how things havechanged the past three years! Back in the olddays you could eavesdrop on their every move -in fact, an acquaintance I know of avoided a bustentirely because of scanner monitoring. But theyare more careful about what they say over theairwaves now. And Motorola now manufacturesdigital encryption equipment that provides live,real-time scrambling of their most sensitivecommunications. Even more unfortunate for theclandestine operator are the recent

    advancements in Low Probability of Interception(LPI) radio. One of these LPI advancements is"spread-spectrum" radio. In this mode the radio'sfrequency changes randomly several times persecond across a wide range of frequencies -even across an entire band! The receiving radioknows which frequencies to constantly switch tofrom a random seed number that is sent theinstant the microphone is keyed. This technologyis the future of government radio. Perhaps incombination with digital encryption it may verywell be the ultimate in airwave security. AnotherLP I technology is "trunking." This mode

    resembles cellular telephone technology in thatthe radios hop from frequency to frequencybased on their proximity to numerous antennas

    spaced across the locality. And like cellularphones, they put out very little power (usually lessthan one watt). So unless you are close to theunit, you will not hear it.

    But I told you I was listening to them as I wrotethis. How? Well, several big problems remain for

    government agencies. First is money. Thisdecade is one of declining budgets and tighteningof belts. Spread spectrum radio equipment is veryexpensive, and it takes a highly trained (andhighly paid) technician to install, program, andmaintain it. Even Motorola's digital encryption(DES/DVP) equipment is expensive, and costly tomaintain. Trunked radio systems are cheaper,and they are somewhat harder to intercept thanstandard equipment, but they must maintain closeproximity to their antenna network, and they canbe monitored most easily if they are in closeproximity. This allows the clandestine operator

    not only to monitor their transmissions whenclose to your lab (the most important time to listenanyway!) but also to determine when they areclose to your operation (even if scrambled). If youhear encryption on a trunked frequency, I wouldstart flushing quick!

    I definitely hear more encryption, but surprisinglylittle for how long the technology has beenavailable. Encryption sounds like unmodulatedstatic for the length of the transmission, followedby a short high pitched "beeeep. Interestingly,they often encrypt only one side of the

    transmission. Often too, they don't seem to knowtheir encryption mode is not on. Coupled with avoice activated tape-recorder (these cost lessthan 50 dollars) you are provided with a concisesynopsis of their daily communications andactivities, the portion you are monitoring, that is. Ihighly recommend scanners.

    Most DEA radio activity will be found between418 and 419 MHz. They also operate some in the162.5 to 163.7 range. I have heard them a coupleof times in the 417.400 to 418.000 range. IRSand other federal agents like to hang out around415 to 418 MHz. Most good scanners allow youto search between an upper and lower frequencylimit. The trunking radio systems, which really arenot very common, will be found above and belowthe standard cellular telephone frequencies. Mostlarge cities (even many small ones) have ascanner monitoring club that publishes a listingfor that area. Such a list is a good place to start,but remember that the Feds change theirfrequencies often and it may not be up to date.One nice thing is that scanner monitoring is aperfectly legitimate (and popular!) hobby - there'sno need to be shy when asking questions down

    at the local radio store. Most scanner buffs areconservative, upstanding, voting citizens! Reallygood scanners have a "search and store" feature

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    that compiles a database of activity and thefrequency it occurred on - all while completelyunattended!

    My recommendations for scanners? Good basicunits are Radio Shack's higher end "Pro-" series(the "PRO-2006, "PRO-43," etc.). They scan fast,

    and cover the new 800 MHz band. They go onsale often for 100 dollars or more off. For a bitmore money, the Ace AR-2500, at 500 dollars isan excellent radio. It receives everything fromshort-wave to 1500 MHz... no gaps. And it has anRS-232 port on the back. This allows you to hookthe unit up to a personal computer and do suchthings as search and store and logging. Forinstance, when the scanner stops on a specificfrequency, your computer screen can instantlylog the frequency/date/time/length of thetransmission, tell you if you've heard stuff on thisfrequency before, and if you have, display any

    notes (example: "DEA ch. 2, local Los Angeles")you have on it.

    Also good, though a bit dated, is the ICOM R-7000. It has a built-in search and store mode, notrequiring the connection of a computer (althoughit has an RS-232 port should you want one forsome of the bells and whistles mentioned earlier).

    A base antenna mounted outside is a must. Youwouldn't believe the difference you'll notice fromthe telescoping antenna that comes with mostradios. Base antennas are cheap less than 20dollars), and you should mount it as high as youcan without it being obtrusive. I have minepainted dark flat brown and stuck up in a tall tree.It's invisible even when you're looking for it.

    Whatever you decide to do, don't ever let yourscanner give you a false sense of security.NEVER assume that you are hearing all there isto hear; you most certainly are not. Use scannersas just another information gathering tool in yourquest to take the fewest risks you can.

    Safety

    Dangers inherent to organic chemistry cannot beignored. An accident is an excellent way to drawattention (from friends if you're lucky, from thepolice if you're not).

    Strong acids and bases can severely bum skin.They can also easily blind you. Safety gogglesare cheap insurance against the loss of yourvaluable eyes. Neoprene gloves offer excellentprotection from most chemicals. If you have largeamounts of concentrated acids, bases, orreactive reagents, transfer working quantities intosmaller containers for use in your immediateworking area. If a procedure requires a dilutedsolution, perform the dilution away from otherchemicals. Be very careful doing reduction

    reactions with chemicals like lithium aluminiumhydride. When a procedure calls for themaintenance of a low temperature or an inertatmosphere, don't compromise! Hydrogenperoxide, especially above 20% concentration, isextremely harmful to your eyes. Concentrated

    ammonia is also dangerous. It can often bereplaced by another, less noxious base, likeNaOH or KOH.

    Ether seems to always present dangers in aclandestine lab. Learn to respect this highlyvolatile solvent. Its vapors are heavier than airand can travel downwards to an ignition source.Eliminate all sources of sparks in the area.Florescent lamps, thermostats, telephones,motors, clocks, non-mercury switches, breakerboxes, and relays are notorious sources of etherignition. The thermostats on many "laboratory"hot-plates spark. Steam baths with a remote

    source of steam are the safest source of heat ifyou're using ether. Never store ether in thefreezer or refrigerator to retard evaporation! Thesparks from the fan or thermostat will cause aviolent explosion. Even static charges can triggerignition. (There are very expensive, speciallydesigned freezers for storing flammable solvents,but I won't get into them here.) All conduit, cases,and metal housing should be well grounded. Afume hood is a must for this solvent. Be verycareful around ether, if you really must use it atall. It can often be replaced by methylenechloride, chloroform, methyl ethyl ketone, or

    others as a reaction medium. Its high volatility,sweet aroma and low toxicity make it best suitedas a final rinse for many drugs.

    Acetone is another popular, flammable solventthat most labs find it hard to be without. Acetonecan sometimes be ignited by travelling throughthe air at high velocity. For this reason, neverpour it through the air from a high distance. Evenmore dangerous is pumping it from one containerto another and letting it fall into the bottom of a 55gallon container. This is especially pertinent tolarge scale operations. Whenever trucks or

    railroad cars are filled with acetone, they arepumped with a tube that extends all the way tothe bottom of the tank so that no solvent fliesthrough the air. My pals at the solvents supplyhouse educated me about acetone. Veryflammable.

    A few more suggestions: use pull ties to secureloose cords you might trip over. Never leave aheating operation unattended, especially duringevaporation of solvents. And, keep a good fireextinguisher near by and keep it charged.

    I doubt seriously if clandestine labs contribute

    significantly to global pollution, but you canreduce the impact to your own yard and watertable. Large manufacturing companies dump all

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    their crap into rivers or leaky underground tanks,or they bribe public officials. Fortunately, as arelatively small operator (compared to say, Bayer)you do not have to use these measures. Themedia loves to pump up the public's anger whenthey show drug lab busts on m. They zoom in the

    cameras on a spot of dead grass and say, "Theowner of this lab dumped acid and toxic poisonson the ground... just 500 feet from where yourchildren play!"

    Always neutralize your waste with lye or muriaticacid (whichever is appropriate) to pH 7. If youhave both acidic and basic wastes, considerusing them to partially neutralize each other (thenuse lye or acid to finish). Using a rotaryevaporator, or even a simple, home-made "still"can greatly extend the use of your solvents. Itsimply makes no sense to set a volatile solventoutside to evaporate when you could dry it faster

    with a still, AND recapture pure, clean solvent foruse again. You'll spend less money, breathefewer fumes, and make fewer risky trips to thechemical store. Reclaimed solvents are as good(often better, more pure) than new ones

    Safety is not only critical for the prevention ofinjury. It's also important for maintaining secrecy.Think ahead!

    Location and Facilities

    Most of us lack the financial resources required to

    construct an ideal laboratory. A large commercialbuilding with a basement on a 300 acre secludedlot would be great. As likely as not, yourlaboratory will be a compromise between what isavailable and what you can afford.

    Basements are wonderfully suited. Water anddrain lines are easily accessible. Walls and floorsare usually concrete, which is non-flammable andeasy to keep clean. Basements are also easilyconcealed from the rest of the building or house.Persons unfamiliar with the particular buildingmay not even know a basement exists. Theentrance door can be made to look like an

    ordinary closet (with a lock on it, of course).Sounds are deadened.

    Windows are usually minimal. And security isusually easier.

    With careful planning, however, you can put a labnearly anywhere. Security and safety are ofcourse the primary concerns when looking for alocation. A large, walk-in closet could even work ifonly small quantities were being dealt with. Agarage is good too, provided you have privateaccess. Whatever the location, be certain ofseveral things before you begin or sign a lease.First, that the area is accessible only to you. Don'tlocate the lab in a place others will walk through

    to get to circuit breakers or other areas. Be surevisibility is impossible from any window, angle,hole, door, etc. Make certain that adequatearrangements are made for the safe andthorough removal of fumes and odours. Becertain that running water is available (a 5-gallon

    jug of distilled water can be elevated above thework area and tapped with a siphon). Also, havea toilet (or large drain with water supply) nearbyto dispose of products in an "emergency." Last,be absolutely certain you can lock up the labsecurely while you're not there, and while you'reinside working. Ample room is nice if you canhave it. I once constructed a small laboratory inthe pantry of a tiny bathroom. It was wellorganized and even had a fume hood built intoone of the shelves. I tripped over one of thepower cords, jerking a hot plate and beaker ofnearly completed product to the floor. This lab

    never produced a gram of usable product. Don'tcrowd yourself.

    I particularly discourage anyone from putting alab in an apartment building. Thin walls,neighbours on all sides - it just doesn't makesense. Locate a house, a farm, a smallcommercial building, a workshop or some thingsimilar if you plan to do any serious work.Commercial property has an added plus in thatyou can blend in easier. In any city's industrialdistrict there are always people loading andunloading drums, creating foul odours, andworking late hours. I must admit, it's hard for me

    to enter any establishment without envisioning itsuse as a clandestine lab. I often enter places thatcould easily be making drugs right in front of meand I'd never know: people carrying bottles anddrums, horrid smells, etc. These places operateevery day of the week, year after year, and noone questions a thing. There is no reason youcan't operate a clandestine lab with a similarfacade.

    Wherever you choose, always rent or lease. It willbe confiscated from you if you're busted and youown it. And never pay your landlord in cash, it will

    arouse suspicion. Get a bank money order fromthe same bank each time and pay at the sametime each month. You'll be in like Flynn this way!

    When to Stop and How

    Someone once asked me if I had ever come"close" to getting caught. This doesn't normallyhappen unless you're very lucky. If you aresuspected of illicit manufacture or distribution,you are investigated and apprehended as soonas possible. Since the first edition, there seems tobe less and less required to obtain a judge's grant

    of a search warrant. Such "evidence" can evenbe a lie from an informant they've cut a deal with.

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    If you make a consistent effort to eliminateevidence of all types, you'll have no regrets.

    Several years ago I made the mistake of workingwith a partner who had "less than sealed" lips.That realisation came when I was approached bya third person who claimed they heard I was a

    "chemist," and asked if I knew of a "recipe" forcrank. That was the time to stop, and I did. I waslater able to bring that bad "rumour" to an end.

    If anyone but you becomes involved or informed,it is time to stop. If you are working with apartner, then things are a bit more complicated.Regardless, if you ever hear something aboutyourself from someone you didn't tell it to, a bigred flag should stand up! If you're asked anyunusual questions by anyone that imply"chemical manufacture," consider stopping Ifneighbours complain of bad smells, stop. If your

    precursor shipment was accidentally signed forby someone who knows your real identity (i.e., aneighbour), stop. If your answering service getsodd calls, stop. If just about anything happens,stop! Get rid of any products (which youshouldn't have around much anyway), wash upglassware and equipment, and lay low a fewmonths.

    History tells that too few clandestine chemists dostop. Many get right out of jail and immediatelystart manufacturing again. I know of numerousindividuals either on the run or incarceratedbecause they didn't stop - most of them in spite ofblatant warning signals. Either proceed with youroperation flawlessly or pack up. If someone is onto you, it's just a matter of time. This is the voiceof experience.

    It's a also a great idea to stop frequently anyway -even when things seem to be going well. Anongoing, continuous operation is usually a timebomb.

    Glassware

    Never keep academic papers or chemistry books

    of any kind on your property if you are making"stuff". Memorise. Try to use anything butcommercial glassware if you can. A surprisingamount of chemistry can be done with spaghettisauce jars and various types of tubing. Evenholes can be drilled in spaghetti sauce lids andbrass pipe fittings soldered, for variousoperations involving gases.

    For example, I performed the entire synthesesusing nothing other than sauce jars and a largePyrex juice dispensers as containers. One saucejar has two fittings attached to it so that an outlettube for gaseous reagent could be attached, plusan inlet for air from a fish tank bubbler. The Pyrex

    juice dispenser was used to contain the etherealsolution of another reagent.

    Though you can (and should) use almost anyglass containers, you will probably need topurchase a few scientific glassware products.This is the major expense of a laboratory, as

    most persons lack the expertise to construct suchequipment. A good glassware kit is essential. Itenables you to efficiently distil substances underreduced pressure, and monitor precisetemperatures. These capabilities are essential.Vacuum distillation is a far cry from boiling offunwanted components in a saucepan using ameat thermometer. The typical glassware setalso contains equipment to accurately addcontrolled amounts of one component to another,under inert conditions if necessary. Undervacuum, solvents and reagents can be quicklyevaporated and the fumes discharged in a safe

    manner. Good glassware also facilitates theseparation of needed chemicals fromcommercially available products (this isdiscussed in more detail later). High qualitydistillation equipment is the centrepiece of a druglaboratory. This is even more important now thanwhen the first edition was published, because ofthe unavailability of many chemicals. Gooddistillation equipment permits the recycling ofsolvents, sparing you the high-risk affair ofpurchasing large quantities of solvent.

    Glassware required:

    25-1000 mL. flasks,Vacuum Adapter,Gas Inlet Tube,Separatory Funnel,Thermometer Adapter,Ground Glass Stoppers,Distillation Column,West-Condenser,Claisen Adapter,Connecting-Adapter,Thermometer.1000 mL 3-neck & 2-neck flasks500 mL 3-neck 2-neck flasks

    For typical set-ups for syntheses consult anorganic chemistry lab manual.

    Reflux. This setup is used for reactions whichmust be gently boiled for long periods of timeEvaporated liquid is returned to the boiling flask

    Simple Distillation This setup is used forpurifying solvents and rapid separation ofcomponents with widely differing boiling points.

    Steam Distillation.This is widely used forseparating volatile oils from plant material The oil

    comes over with droplets of condensed water inthe receiving flask

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    Reflux with additionThis popular setup allowsthe controlled addition of one liquid to another.while monitoring temperature. An inert gas suchas nitrogen is often bled in from the 3rd neck. ifneeded a magnetic stirrer is often used as well.

    These glassware kits are available from many

    laboratory supply outlets. I've also seen them atparaphernalia smoke-shops at outrageous mark-ups. Obtain the universal type, with ground glassjoints. If you can't find one, browse a currentjournal (at the library) on "laboratories." You'll findads from glassware manufacturers as well assources of other equipment you may wish toinvest in. The Thomas Register is anotherexcellent place to look, and nearly every libraryhas it. Obtain an accurate thermometer for usewith the glassware set. Be certain you know thesubmersion it was designed for. Seventy-fivemillimetres (75 mm) is needed for doing

    distillations on most glassware sets. This is veryimportant: a "total immersion" thermometer willgive false readings if not fully immersed.

    In addition to this universal kit, you will probablywant to add a larger size boiling flask, say 1 L or2 L. Both are even better. You'll also want alarger separatory funnel. Large sep. funnels areexpensive. A solution to this dilemma is to shakesmall quantities of the mixture in the small funneland transfer them to a converted jug.

    For powerful solvents, like tetrahydrofuran,methylene chloride, or acetone, you'll probablyneed a glass jug. Glass lugs of one galloncapacity, and glass water jugs of 5 galloncapacity (carboys) make excellent largeseparatory funnels. The bottom of thesecontainers is cleanly cut off as follows: (seeFigure opposite) the jug is "scored" with a metaltriangular file several inches. The score should bestraight (use tape as a guide) and extend about to the way through the glass. A piece ofnichrome wire, available at hardware stores, ispulled straight (if coiled) and wrapped tightly oncearound the jug, passing precisely on top of thescore. Overlap the wires slightly (but don't let theends touch!) so that no gap remains, and applycurrent to the wire. You can either plug it directlyinto 110 volt house current or: run it through apower-stat. The wire will glow red hot and almostinstantaneously you'll hear a soft "tink!" Thethermal shock will make a remarkably cleanbreak. If it doesn't work right away, remove thecurrent, make the score longer, and try againafter the glass cools.

    A carboys, wine bottles, and other glass jugscan be easily cut to make large separatoryand filtration funnels.

    B Using tape as a guide, score a notch severalinches long. It should extend about of the

    way into the glass. A small triangular or flat fileworks well for this.

    C Wrap the entire circumference with one turn ofnichrome wire, crossing directly over thescore, use tape to secure if necessary, wiresshould come close but not touch! Take your

    hands off the nichrome wire and apply power.The wire should fit tightly against the jug whenit heats up.

    D The end will usually break off cleanly the firsttry. If it doesn't, make your score a little bitlonger and try again.

    E With a stopper and valve fitted to the mouth,these jugs make good separatory funnels. Usea stirrer for mixing. Use a gallon jug (glass orpolyethylene) with bottom cut out. This has ametal tube brazed to jar lid (if metal). Caution:excess heat will destroy thin lid!

    Connect metal to glass with small piece ofrubber. polyethylene, or Teflon tubing. Use aglass tube to view separation point. To controlfluid flow use a pinch clamp on tubing or valveGlassware

    F A perforated metal, glass, or polyethyleneplate epoxied into the bottom makes a largefilter funnel.

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    This procedure is remarkably reliable, and is infact how commercial glass workers cut largetubing as a matter of course. Sanding with siliconcarbide sandpaper will make the sharp edgesmooth, if desired.

    Turn the jug upside down and you now have a

    large funnel. You'll need to put an operable drainon the bottom (which was formerly the top). Thiscan be a tight-fitting rubber cork with a glass tubeand a pinch clamp, or you could use epoxy puttyand fit a stainless steel ball-valve. You'll alsoneed to make a stand for it. Larger sizeseparatory devices are discussed in the scalingup chapter.

    [Editors Note you dont need to use a carboy tomake the filter. A filter funnel and bowl with a flatbottom, made out of PP or HDPE, will be mucheasier to work with. A pattern of holes is drilled

    into the bottom of the bowl which is then gluedonto the filter funnel. If you use a carboy as thefilter flask be sure to cover it with thick clearplastic sheet so that if it collapses under vacuumstress you wont have broken glass flying intoyou.]

    For containment and storage purposes, regularglass jars make excellent beakers. Glass salad-dressing and BBQ sauce bottles, as well as jugscan be used in place of Erlenmeyer flasks. Thelarge, 5 gallon glass water carboys areindispensable for storing large quantities ofcorrosive chemicals. Get into the habit of savingglass jars from the foods you consume.

    A wonderful (and expensive) luxury is a "rotaryevaporator." These devices take the hassle andwait out of evaporating large quantities ofsolvents. They spin the boiling flask in a hot waterbath under vacuum, making the solvent spreadover the entire inside surface of the glass. Thisincreases surface area, and reduces violent,erratic boiling. They have large condensers thatquickly recycle solvents into an easily removablereceiving flask (to be reused of course).

    Courses in glassblowing used to be required inevery chemistry curriculum. Up until 50 yearsago, chemists were expected to make all theirglassware. Nowadays, this skill is confined to asmall handful of specialized, professionalglassblowers. Every now and then, a course inglassblowing is offered at some communitycolleges. If you find one, sign up for itimmediately! Skills in rudimentary glass workingare priceless to the clandestine chemist -especially with the crackdown on sales oflaboratory equipment. An excellent book onelementary glassblowing is Creative

    Glassblowing: Scientific and Ornamental, byJ ames E. Hammesfahr and Clair L. Strong. Thisinexpensive book covers everything from the

    basics to making exotic scientific apparatuses.The tools required are minimal.

    Even if you don't "blow" glass, you can get a fewassorted pieces and bend them with a propanetorch to make simple stills and condensers. Getsoda lime glass to Practice with. All laboratory

    ware used to be made with this glass before thedevelopment of "hard" borosilicate glasses. Sodaglass can't take extreme thermal shock, but youcan work it with an ordinary propane torch. Pyrexis great stuff but you'll need an oxygen-enrichedflame to soften it. You can also buy pre-madeground glass joints and stopcocks. These makethe fabrication of many items simple. BethlehemApparatus Company in Hellertown, PA sells allkinds of glass working tools and kits. Bulk glasstubing, rods, and pre-blown flask blanks can befound inexpensively in the Thomas Registerunder "glass.

    Heating, Stirring, and Mixing.

    This sort of equipment is perhaps the easiest andmost economical to construct. Heating mantlesare easily constructed using nichrome heatingelement wire and a suitable cement. Asbestoscement is great. It's also nearly impossible to findsince the carcinogenic properties of asbestoshave been publicised. Refractory (fireplace)cement or mortar is available from buildingmaterial and hardware stores. It makes a fairlygood substitute. You can also use "kiln" mortar,

    available from some art supply and ceramicsstores. In a larger city, look in the yellow pagesunder "refractory. Here you'll find manybusinesses that cater to those who use hightemperature equipment and Supplies. They haveexcellent materials for the construction of heatingdevices, including glass wool, high temperaturetapes and adhesives, and a variety of cements.These places also sell fireproof sheets of rigidboard (Transite, Marinite) that make excellentliners for fume hoods.

    Heating mantles can be made several ways.

    You can either start by packing the cementaround the flask, or by pressing the flask into amold filled with the cement - see Figure. A plasticmargarine dish works fine for the latter. The flaskcan be removed as the cement begins to harden,and the nichrome wire pressed into the surface ofthe cavity. The flask should then be placed backinto the cement as it shrinks during the dryingprocess. Use large brass screws pressed into thecement to connect the nichrome wire to thepower cord. The heat can (and should) becontrolled by a variable transformer (power-stat).Be certain it is capable of handling the wattage

    consumed by the length of nichrome wire youhave selected. Use a moderately long cord on theheating mantle to place the power-stat away from

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    any flammable fumes. Make sure the connectionsof the cord to the mantle are tight. A coat ofparaffin on the flask will facilitate removal. Betterstill, is a "mold release compound." There areseveral types, any of which will work. The best forthis purpose has graphite in a water based

    suspension and comes in a spray can. Look forthese release compounds at art supply storesand businesses catering to those involved withceramics and casting.

    Some typical heating mantles

    A heavy brass screws are set in cement toconnect unit to power-stat,plastic dish used as temporary mold forcement

    B bottom of coffee can is used for support withoptional insulation to isolate the nichromecoiled heating element.

    C nichrome coiled heating element is set intorefractory or fireplace cement with a jar orbeaker for support during drying.

    Coat the bottom of a round bottom flask withparaffin or, better still, with a slurry made frompowdered pencil leads and enough H2O to makea brushable paste.

    A mechanical heat control can be a source ofsparks!

    Detail of thermostat: most inexpensive units havea bi-metal, open contact device that shrinks andexpands with the temperature. If you're usingflammable substances, solder this contact closed

    (or remove it completely) and control thetemperature with a power-stat of suitable size.The power-stat can be located outside your fumehood. Also solder any switches or replace withsparkless mercury types.

    Small hot plates can be made sparkless bysoldering the internal thermostat closed, andusing a power-stat of suitable size to control theheat (See Figure). Of course, if you are notworking with flammable fumes, there is no reasona regular hot plate won't work.

    Don't underestimate a steam bath. They are

    excellent laboratory heating devices. Theyproduce very even heat that never exceeds 100

    o

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    C. This is perfect for drying residual traces ofwater and solvent out of your Product undervacuum. Steam baths also produce no sparks,and are excellent as a heat source for distillationof low-boiling point solvents.

    A The simplest steam bath can be made from a

    coffee can. It has a hole cut in the top slightlysmaller than the flask to fit in also a small holein side for excess steam to escape. The unitis filled to full of water and heat is appliedto the bottom.

    B A steam source could consist of a pressurecooker with a copper, brass, or stainless-steel tubing brazed or soldered on the tophole. An optional valve can also be present tocontrol the steam flow in the steam line. Don'tremove any relief valves which are needed torelieve excess pressure.

    C copper, brass, or stainless-steel tubing canbe brazed or soldered to top of any strongcan. cut inch hole in can and shake outcontents. Provide a steel or brass plug forfilling this hole.

    Steam baths are easily made using a low profilecoffee can. (see Figure) Cut a hole in the top withtin snips. Make it large enough to allow thedesired submersion of the flask or beaker. Asteam generator can be made by adapting apressure cooker or a heavy metal can of mostany type. A wall-paper stripper unit makes anexcellent steam source.

    Pipe heating tape can supplement anotherheating device, and is useful in somecircumstances. These are sold in building supplyand hardware stores for the purpose of thawingfrozen pipes. Most of these tapes have a built-inthermostat that allows operation only below 35degrees F. Solder the thermostat closed andcontrol the heat with a power-stat. Pipe heating

    tapes are quite versatile as they can be wrappedaround any size or shaped vessel. They do nothowever, provide the even heat of a good heating

    mantle. Unless you obtain one made from glasswool or asbestos, they are not suitable for hightemperatures.

    Though a bit messy, oil baths are the method ofchoice for many heating applications, and theyare easily constructed. The high temperature is

    evenly dispersed over the vessel, eliminating hotspots that cause excessive bumping andfoaming. You can instantly control the heat byvarying the immersion of the vessel. These bathscan be constructed by simply placing an oilcontainer over the heat source.

    Another method is to place a nichrome heatingelement directly into the oil and use a power-statto control the heat. Several loops must be madein the nichrome. A candy thermometer can beclipped to the side to indicate the approximatetemperature of the oil.

    The deep fryers sold in department stores makeexcellent oil baths. They are compact andtransfer nearly all of their heat into the oil. Theirinternal thermostats make sparks, but you canbypass the thermostat and use a suitable power-stat if you are using it around flammable vapors.For temperatures up to 200

    ,C mineral,

    vegetable, or peanut oil are suitable. For highertemperatures, use silicone oil. Silicone brake fluidmakes a substitute after some of the lower boilingadulterants smoke off. Oil baths are well suited todistillation, as they provide a constant, even heat.

    With any oil bath, be certain to support the oilcontainer and other related equipment well. Hotoil all over your legs can ruin your whole day!

    Avoid Bunsen burners and other open flame heatsources. They not only supply a source of ignitionfor fumes, but distribute their heat unevenly. Thissharp concentration of heat in one spot cancause glass to break from thermal shock.

    [Editors Note: An inexpensive heater for an oilbath is to use 125 ohm, 5 watt resistor. This is

    place directly into the oil bath.]

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    Distillations seem to give many readers lots oftrouble. Here is my method for hassle-freeoperations in this endeavour: Keep the quantitysmall. A 2000 ml flask is the largest you shoulduse for most procedures. A 5000 is the absolutemaximum, and only for low-boiling liquids. Always

    use a heating mantle, rather than an open flame.A flame heats one single hot spot on the flask,this makes the boiling quite violent. A heatingmantle (either home made or purchased)provides a steady, even heat. You can evenblanket the top half of the flask with glass wool formore effective retention of heat. Stir the liquidduring the distillation. This makes a remarkabledifference! The distillation proceeds faster too.The easiest way is with a heating mantle placedon top of a magnetic stirrer. Some commercialheating mantles have a magnetic stirrer built in(expect to pay around 600-800 dollars for one of

    these gems in the 2000 mL size). Another way isto use a 2 neck flask and have a glass or Teflonstirring rod enter through the second opening.You can either stir with your hand (the poor man'smethod) or you can use a stirring motor.Whichever way you go, you'll be amazed at howmuch improved your distillations are when donefollowing these guidelines.

    Stirring and mixing equipment are easily obtainedat second-hand and thrift stores. Garage salesare good too. Old metal blenders costlaboratories hundreds, but they are easy to findsecond hand for a few dollars. The old milkshake

    mixers are great for quick immersion into a flaskor beaker - a great aid when trying to get somesolid powder into solution.

    Magnetic stirrers can be easily made from aturntable or tape recorder (small AC inductionmotor) motor and a coffee can mounted onrubber-feet. The top consists of a plastic lid, orbetter inch aluminium plate. You can use aceiling fan speed control on some of thesemotors, but others require the speed-controllingmechanism in the original device. You might findit convenient to mount the speed controller in the

    base of the unit. The mains cable is insulatedfrom the can with a plastic or rubber grommet.

    Wadded up chicken wire or a coat-hanger servesto hold the motor in position while the foamsealant dries. Foam sealant adheres vigorouslyto all surfaces and eliminates the need forcomplicated shimming and mounting hardware.Epoxy putty, used by plumbers, is an excellentalternative. It hardens to rock hardness in about 5minutes and can be moulded like clay. This greatstuff has many uses in the construction oflaboratory equipment.

    You can purchase stir bars or make your own bysealing a bar magnet into a heavy polyethylenedrinking straw (or tubing) Seal the ends with a hot

    iron or melt them shut with a small flame You canalso use glass tubing, if available.

    It's probably best to purchase stir bars. TheTeflon coated type is inexpensive and available atscientific supply companies. You can, however,make your own stir bars from sections of

    polyethylene tubing (the opaque white variety) orthick drinking straws. Melt the ends shut around asmall bar magnet. You might even make a"spinning ring" by moulding a ridge around thecentral circumference while the tubing is soft.This feature is found on commercially made stirbars, and is especially useful for stirring largecontainers with irregular or rough bottoms.

    For stirring thick slurries or viscous reactions youwill need something more substantial than amagnetic stirrer. A direct drive or "wobble" stirrerserves this purpose. These stirrers are used in

    the synthesis of the DMT class of drugs, whichform a plastic-like intermediate. Don't be misledby the illustration of the wobble stirrer. Your firstreaction might be: "Hell, man, Ill just stir it withmy hand." But reactions often take hours, andvigorous stirring over the entire period is essentialif good yields are to be expected. Constructiondetails of a wobble stirrer are shown in below.

    Unless your motor is very small, a reduction is notnecessary. Again, a ceiling fan speed control canbe used to vary the speed of most small inductionmotors. If necessary, a small piece of bicycleinner tube can be stretched over the mouth of theflask (the protruding part tucked inward) toprotect it from the vigorous movement of the stirshaft. Polyethylene tubes to enclose the stir shaftcan be obtained from a "Winder" or other spraybottle. A wooden frame, finished with marine

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    varnish has a small induction motor attachedwhich rotates a round wheel of steel, wood,plastic, etc. The stir-bar is a polyethylene tubewelded over a rod and sealed inside for stiffness.

    The round bottom flask must have a short neck.Heating is provided by a heating mantle

    (nichrome wire embedded in cement with screwterminals for connection to power-stat).

    Shown in the figure above is a simpler model thatcan often suffice. It does not vibrate the flask orslosh as violently as the wobble version.

    This alternative stirrer is easier to construct andworks just as well for many applications. A or3/8 drill chuck is attached to a motor and ~

    polyethylene or stainless steel rod has a hingedpaddle so it fits through mouth of the flask. To fitthe paddle file notch in rod for paddle and secureit with stainless steel rivet or pin.

    Certain flammable solvents can be used withcaution in sparkless mixers such as a blender.Ethanol is okay, especially if diluted with somewater. This is done all the time in bars whenmixed drinks are made. This procedure isfrequently called for when you must grind up acrude plant product prior to extraction. Never dothis without good ventilation, and never use ether,

    acetone, or similar highly volatile solvents. At thevery least, use the setup with a large plastic bowlconnected via a flexible tube to an extractor

    motor. This acts as a hood for extracting fumes.Much better of course is to perform the entireoperation inside a fume hood with the blower on.

    I've mentioned several terms in conjunction withmotors in this chapter. I'd like to discuss brieflythe various types of motors and clear up some

    confusion that Often arises. AC Motors fall intotwo broad categories:

    Universal AC/DC (with brushes) and brushlessinduction motors. The first type is usually found insmall power tools like drills and saws, and hasthe advantage that its speed can be easilyadjusted by use of an inexpensive speed control.Its major disadvantage for the laboratory operatoris that the brushes produce sparks that willquickly ignite flammable vapors. Brushlessinduction motors as a general rule produce nosparks. They are divided into several types:

    "open drip proof," "totally enclosed fan cooled,"and "explosion proof." An explosion proof motorproduces no sparks and it must by definition beable to withstand an internal explosion.Furthermore, it must not allow the internal flameto escape. Be sure you really need one of theseexpensive motors before you go out and buy one.You can usually eliminate their need by keepingmotors out of the area when you use flammablesolvents. One place you might consider one is inthe exhaust fan of your fume hood, but that willbe discussed in detail in the next chapter, onfume hoods. Induction motors have the

    disadvantage that it is difficult to control theirspeed. They rely on the frequency of theincoming line (60 Hz) to establish speed. True, aceiling fan controller can control some smallinduction motors, but you'll quickly overheat mostlarge ones.

    Fume Hoods

    Fume hoods are very important to the clandestinelaboratory operator. Most importantly, theyprotect you from toxic material and flammablevapors. However, they also allow the efficient

    removal of suspicious odours from your vicinity.Thick sheet-rock is an acceptable material forconstruction of fume hoods, provided it is paintedwith several coats of epoxy paint or marinevarnish. Sheet-rock is flame retardant, cheap,and easy to work with. Wood or metal sheet-rockstuds can be used to reinforce the sheet-rock ifdesired. Use caulk or joint compound to seal theseams up well. Wood can be used as well,provided you line the interior with "stove-board,"refractory board, or sheet-rock. In fact, any largewooden box can be used provided you protect

    the interior. Asbestos board is unavailablenowadays, but the ceramic fibre replacementsTransite, Marinite) make excellent building

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    materials for fume hoods. Figure 16 shows thedimensions for a suitable hood from standard 4 x8 foot stock. You will have to trim the edges toallow for the thickness of whatever material youselect. Placement of the baffle is important: oneinch off the bottom and two inches from the back.

    These dimensions produce a hood of theminimum recommended size. A hood about 5 feetwide is the ideal size.

    A 4' x 8' sheet-rock (heat resistant) or plywood isused. The back is 2 x 3, the sides 1 x 3; thetop & bottom 2 x 1.

    A more elaborate fume hood shown has twosliding doors: a clear sheet of " Plexiglas andan outer solid door that locks closed. I built thishood in a tiny garage and it was a complete joy towork with. The Plexiglas was lowered to within 10inches Or so of the work surface so I could reachin with my hands to work. A light inside providedperfect visibility to an odor free work area, and I

    was protected from any exploding debris by thePlexiglas. A Halon fire extinguisher was keptmounted nearby and could easily extinguish amajor fire in this enclosed, fire-proof space. Whennot in use, the outer door slid down and locked,completely concealing the contents. It actuallylooked just like an ordinary workbench when itwas all locked up. I strongly recommend you doyour chemistry in a hood similar to this. It willlower your risk factor significantly.

    A small bar sink is useful mounted inside one ofthese hoods. You can then have your aspiratorpump operating under the hood as well. If you'reshort on space, a 5 inch piece of 4 inch PVC pipecoupled to a standard 2 inch drain pipe makes anexcellent cup sink. You can mount it directlyunder a spigot and have your aspirator empty intoit. Most commercial fume hoods have a "cup sink"very similar to this mounted in them.

    A sparkless fan should be used for your exhaustfan. If you really want to do it like commerciallabs, use an explosion-proof blower. With one ofthese, you could safely work a reaction thatproduced hydrogen or acetylene! 100 cfm is theabsolute minimum size. Most large commercialhoods have a blower of about 500 cfm capacity.Figure 18 shows some more details of various

    blowers and their connection to a fume hood.

    Squirrel-cage-type blowers generally make muchless noise than their axial (or radial) counterpartsof the same size. Furthermore, many squirrelcage blowers have the motor mounted outsidethe shroud (good ones even have a weatherproofcover for the motor). This makes the risk ofignition (which is fairly low anyway with abrushless, enclosed motor) even less. Theseblowers are available fairly inexpensively fromGrainger, or a similar industrial supply outlet.These blowers are actually quite unobtrusive

    when viewed from the outside. Drive through abusiness or light industrial district of yourcommunity and you'll see them on just aboutevery building from restaurants to art studios tometal shops.

    The incline type of blower has blades which tiltaway from the direction of travel. This type ofblower cannot be overloaded and usually has themotor mounted in a separate, weatherproofcompartment. This is the standard configurationfor commercial fume hoods.

    If the unit is directly inside the hood the blower

    must be explosion proof if solvents like ether areused.

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    An inline blower is quieter than a blower insidethe hood.

    This inexpensive set up works well. It lacks theflow and loading resistance of the backwardincline unit, but is fine for many applications. Itlooks especially unobtrusive. Be sure to use 12

    inch duct pipe to prevent excess air resistancethat could overload the motor.

    Leave your exhaust fan on continuously so thatno smells ever leave your lab. Don't be the idiotthat tries to tape all the windows and doorsclosed - use an exhaust fan and let the fresh airenter through all the cracks and crevices thatabound.

    For light use a socketless bulb and solder leadsto supply wires otherwise a "vapor-proof" fixturewith thread sealant on all conduit fittings andglass seals can be used.

    In the construction of any fume hood, sources ofignition must be completely eliminated. Makecertain any motors used inside are brushless andproperly grounded. Illuminate the interior of thehood with a "vapor-proof" outdoor fixture orsocketless bulb with soldered leads. (See Figure19.) Mount the switch on the outside of thefixture.

    Run all wires in outdoor-type conduit. The greyPVC variety works nicely and is inexpensive.Eliminate all contact-type connectors such aswire-nuts, light-sockets, plugs, etc. Solder allelectrical connections and insulate them well.Remember, the slightest spark will ignite manyvapors. Keeping the blower on further reducesthe risk as the concentration of any flammablefumes is kept quite low.

    Exercise extreme caution when using ether, evenunder a hood. The flash point of ether is minus20 C. This means that even at this temperature,the vapors tight above the solvent can be ignited.Keep a fire extinguisher mounted to the wall,within immediate reach.

    Another useful device is a movable fume hood,suitable for small operations. Construction detailsof this hood are a polyethylene jar held by theframe from an old drafting light. Flexible ducting issold in building supply stores in a variety ofdiameters. Three inches is the smallestrecommended for this hood. Six inches is muchbetter. This device works well for small projects,but it's no substitute for a full-fledged fume hood.

    The exhaust of your fume hood blower should bechosen carefully. On a commercial building (witha high roof) or farm, you can simply mount theblower on the roof and let it blow the fumes up

    into the air. Use the same trick corporate mega-polluters use to obscure their filth: the higher theexhaust, the better. By the time they reach

    another nose, the odor will be well dispersed andits origin vague. In a house, the vent pipe fromthe hot water heater or furnace can be used andextended by adding additional sections. If thesevents extend high into the air and you are worriedabout being obtrusive with an extra vent, you can

    use them as exhaust ducts. Permanently seal allseams in the vent pipe with high-temperaturemetal tape. (See Figure 21.) A word of cautionhere: be sure the HW heater or furnace and theirpilots are off. To be safe, turn off the main gascock to these appliances if you're usingflammable solvents. This arrangement works wellin a basement where the furnace and HW heaterare often located. The furnace has a much biggervent (6-8 inches) as opposed to the HW heaters(3 inches) and should therefore be consideredfirst. I must stress again that using an existingHW heater or furnace duct is an option to

    consider only if a standard type of blowerarrangement is impossible.

    Fume hoods are really outstanding. Build one andyou'll wonder how you ever did without!

    Also excellent for general ventilation are thosewind-powered turbine attic vents. Though theylack the airflow needed for most fume-hoodapplications, they are great for things like yourstorage cabinets and as a full-time whole labventilator. They consume no energy, are non-sparking, and inexpensive.

    Miscellaneous EquipmentMost additional equipment can be scroungedfrom flea markets, auctions, and garage sales.You may have many items already, but haven'tassociated their use with a laboratory application.Household appliances have the advantages ofavailability, low-cost, and perhaps mostimportant, unobtrusive appearance.

    For non-flammable solvents, an old percolatormakes an excellent extraction apparatus forseparating crude drugs from plant material, oractive ingredients from OTC drugs. Even ethanol

    can be used if cooling is provided on the lid andgood ventilation is available. For moderatelyflammable solvents, the internal thermostat canbe soldered closed and the heat controlled with apower-stat.

    If the percolator is made of brass, copper, orsteel, you can solder a small ring of metal to thelid to hold ice or cold water. Epoxy paste will workif the unit is made of aluminium. In some casesthe lid can simply be inverted and filled with ice. Adry-ice acetone slush will condense virtually allvapors, but acetone itself is flammable. Bags of

    ice can be placed on the lid and these may bereplaced from time to time.

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    Filter paper can be placed over the filter grid tostop power dropping into the liquid below.

    The extraction solvent should be slightly acidicwater, ethanol, ethanol/water, non-flammablesolvents, etc.

    The small espresso pots sold in gourmet coffeeshops are useful for steam distillation of smallquantities (see Figure 23). Steam distillation isuseful for the extraction of volatile oils andterpenes from plant material (such as red oil frommarijuana leaves and resin).

    For efficient extraction of many drugs from plantmaterial, fine powdering of the crude substance isnecessary. Coffee grinders cost much less thanlaboratory mills and work nearly as well.

    Vacuum pumps are a source of much mail fromreaders of the first edition. For some reason,

    people seem determined to make vacuum pumpsfrom refrigerator compressors. In this secondedition, Ill share with you my master plans forcreating a quality vacuum pump from such a unit,but first I'd like to discuss vacuum pumps ingeneral. I still believe the best vacuum pump for achemical laboratory is the simple water aspirator.They're cheap, small, sparkless, don't wear out,and flush residual solvents and odours down thedrain. With adequate water pressure, theyproduce a vacuum comparable to manymechanical pumps. Additionally, aspirator pumpshave a higher pumping speed (about 7

    litres/second compared to 1 litre/minute for aconverted compressor). What more could youask for? This pumping speed is especiallyimportant when evaporating or distilling solvents,as the evaporated liquid quickly expands to fill theevacuated glassware.

    Mechanical pumps are easily obtained second-hand. Look in the newspaper or browse a largeflea market. An old refrigerator compressorcanwork, but chances are the valves are bad. Whywas it removed from the unit for which it wasdesigned? You might acquire an old unit from aworking refrigerator or freezer. Here is my planfor converting such a device into a usablelaboratory vacuum pump: Leave the starting relayin place. This will eliminate the need for atroublesome combination of switches to start theunit. Be careful not to damage the tubes comingout of the compressor. Cut them down to a lengthof about 2 inches. Turn the unit on and identifythe inlet and outlet. Unplug the unit and tip it onits side over a quart sized container so that theoutlet faces straight down (see Figure 24). Let allthe oil drain out (this will take an hour or so), andnote carefully how much oil was in the unit.

    Record this amount, and engrave or scratch itinto the case of the compressor (e.g., oil capacity520 mL.). Tip the unit back up and using a funnel

    replace this exact quantity of oil with high quality"vacuum pump oil." This is available at hardwareand industrial supply stores. You will need tochange the oil on a regular basis (as with allmechanical pumps) to keep the innards of thecompressor healthy. It was designed to run in a

    closed system. Allow the oil to drain down to thebottom and you're ready to go! Be sure to changethe oil frequently.

    Nevertheless, this pump is excellent for certainpurposes, and I wouldn't be without mine foranything. It makes virtually no noise, pulls a highvacuum and consumes no water. It works nicelyfor vacuum filtrations, drying under vacuum toremove trace amounts of water, and small-scaledistillations that don't involve solvents or otherhighly corrosive vapors. Don't use it at all forevaporating solvents or performing distillationswhere large quantities of vapor are produced. It

    will foul up immediately. If you allow the unit torun with the intake wide open to the air, theincreased air flow will blow a fine oil mist out theexhaust. This can be avoided by turning the uniton only when it is connected to your system. Afew units have an oil separator that automaticallyfilters oil and channels it back to the intake. If youfind one of these, all the better, but it's notnecessary. A cold trap should be used on allmechanical pumps to condense any moisture andother fumes before they can enter your pump,though you can do without it if you change the oilfrequently and avoid high volatiles.

    A mechanical pump is a nice accessory, butagain, I think an aspirator pump should be themain vacuum source in a clandestine laboratory.

    To save water, or if your water pressure is low,you can construct a recirculating pumpingstation. This station has been completelyredesigned since the first edition, and this unit'sperformance is truly outstanding.

    You'll still need a source of running water to keepthe unit cool and flush out condensed solvents asthe unit runs. It works quite well, however, and

    the pump can provide a higher pressure thanmost any municipal water supply. Use a 5 galloncan, plastic pail, or something similar to housethe system. The overflow should have a fittingallowing the attachment of a one-inch or largerdrain hose or the unit can be placed in a sink orbathtub. The pump is of the jet pump-type variety,and should be in the range of'/, to M horsepower.Units made for hot tubs and small swimmingpo