Appendixes
Notes on Purity Tests and Precursors
The easiest way for most people to check a psychedelic compound's purity is at a testing station, such as Street Pharmacologist (Box 610233, Miami, FL 33161, 305/ 446-^585), or PharmChem. PharmChem's analysis is based on thin-layer and gas chromatography and involves comparison with 300 possible psychoactive substances and some 250 possible impurities.
Qualitative findings are available from PharmChem two or three days after a compound's reception—if accompanied by S15 by money order or in cash and an identification code of five numbers and a letter, sent to 3925 Bohannon Dr., Menlo Park, CA 94025. The number to call Is (415) 328-6200. Quantitative results are given only to those with DEA licenses.
Chemical test kits advertised by mail order for checking out alleged Psychedelics generally rely on the Keller and van Urk-Smith color-change tests. In these, the sample to be examined is poured into a reagent with the resulting color then compared with standards. Albert Hofmann has described these processes as they relate to LSD:
All derivatives of lysergic acid give characteristic color reactions based on the indole nature of lysergic acid A solution of traces of a lysergic atid derivative in glacial acetic acid, containing a small amount of FeCI^3. when added with concentrated H2SO4 develops a brilliant violet-blue color (Keller reaction). In the procedure of van Urk-Smith a solution of p-dimethylamino-benzaldehyde in diluted sulfuric acid containing traces of FeCl3 is mixed with an equal volume of the lysergic acid derivative in tartaric acid solution. A violet-blue color appears. Whereas the Keller reaction is used mainly for qualitative identification, the van Urk-Smith reaction was standardized and can be used for quantitative determinations.
These test kits are mainly useful in determining whether the substance in question is an indole or not Melting point apparatus is also a rather crude indicator, although valuable as well in finding negative results.
More sophisticated determinations can be made with thin-layer chromatography, a process that is still quite inexpensive. In this technique, the substance to be tested is placed at the bottom of a coated plate and then creeps up through a solvent for ten to fifteen minutes. Various psychoactive components then locate themselves in specific positions and exhibit coloration depending upon the solvent used, and thus can be identified as specific compounds. LSD-25, in a typical reaction, travels about halfway up the gel, where it takes on a bright yellow appearance. The position of iso-lysetgic acid diethylamide, by way of contrast, lies right below. Use of different solvents, while assaying the same substance, can be almost as specific as the results derived from equipment costing $40,000-550,000.
Experience in making thin-layer discriminations is needed, however, since the eventual reading depends upon color distinctions and accurate measurements of resting locations. Gunk from a floor, bits of an eraser, various dyes and even milk have on occasion been thought to have tested out positively by some who have tried
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402 Purity Tests and Precursors
color-change tests. Difficulties in relying on verbal descriptions are evident in Webster's Third International Dictionary's effort at defining onionskin pink:
... a light brown that is stronger and slightly redder and darker than alesan;
stronger and slightly yellower and darker than blush; lighter, stronger and slightly
redder than French beige, and redder, stronger, and slightly lighter than cork . .
A few readers of the earlier edition of this book felt that a revision should contain examples of thin-layer chromatography for most Psychedelics. This, however, would require many precise color plates, and is already available in several versions at many university libraries. Here are examples, in black and white, illustrating typical chromatograms:
E.G.C. Clark's Isolation and Identification of Drugs (The Pharmaceutical Press, London) specifies a method for making "microtests" of a "pedant drop" or "microdrop." The sulfuric acid-formaldehyde testing of DMT, to illustrate, yields dull orange with a sensitivity of 1.0 mcg. sensitivity, while the ammonium molybdate test yields blue going to green and then yellow with a sensitivity of 0.1 mcg.
When asked about other relevant literature on spot color tests. Carmen Helisten, formerly of PharmChem, recommended the following articles:
Fiorese, F.F., "Immediate Drug Detection on the Spot," Hasp. Lab, Set., Vol. 9, #4, 1972, p. 240 ff.; Frank, R.S. et al., "Standardization of Forensic Drug Analyses," /. For. Set.. Vol. 19, 1974, p. 163 ( f-1 Kaistha, K.K , "Drug Abuse Screening Programs;
Thin layer and Gas Chromatography 403
Detection Procedures. Development Costs, Street Sample- Analysis, and Field Tests,"J Pharm. Sci.. Vol 61. #5, 1972, p 655ff...ind Velapoidi, R.A. et al, "The Use of Chemical Spot Test Kits For the Presumptive Identification of Narcotics and Drugs of Abuse," J For Sci. Vol. 19, 1971, p 636 ff
More precise testing is made by column, gas or high performance chroma-tography equipment, or by use of magnetic resonance or an electron microscope. These methods are all quite expensive and necessitate equipment rarely available outside of industry, universities and crime labs.
In gas chromatography, a sample is introduced into an inert stream of gas flowing through a tube. Through heating, it is broken down into its constituents which are then carried by the gas depending upon how heavy they are. Results are evaluated electronically in terms of nuclear weights and compared with an appropriate standard.
High-Performance Liquid Chromatography doesn't involve a heating process, which can alter the original substance. Accessibility to this machine and others even more specific is rare, however.
These matters are raised here to indicate how difficult it is to establish the purity of a psychedelic substance with certainty. Bruce Eisner has discussed issues arising from this situation in "LSD Purity: Cleanliness is Next to Godheadliness" (High Times, January 1977). He has since remarked that
The basic nature of the experiences that people were having with LSD had changed from the early- and middle-'60s to the middle-'70s, with a tendency for people to have less visionary or spiritual sessions and more mundane experiences which tended to remain at the level of simple sensory changes.... It became clear to me that a major factor in the quality of LSD reactions was due to the decline in
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the chemical purity of the substance itself. The deterioration of purity did not refer to chemical adulteration, but rather to the faulty manufacture of LSD by underground chemists, leading to a product which was not chemically pure crystal LSD but LSD mixed with a number of by-products of faulty manufacture. The source of impurities, exposure of LSD crystal to light, heat, moisture, air and combinations of these common environmental conditions deteriorate even the purest LSD into an odd collection of chemicals
Four factors—set, setting, ^uide and dosage level—arc .ill explanations m the changing receptivity to LSD in the psychedelic subculture. Pharmaceutical purity, a fifth factor, may play an important part in the overall variability of LSD experiences. At least, this question should be the subject of more thorough scientific research.
As for the synthesizing of Psychedelics, Loompanics Unlimited, the publisher of Michael Valentine Smith's 1981 version of Psychedelic Chemistry, offers an appropriate warning: "The procedures referred to and described in this work assumes thorough knowledge of advanced lab techniques in organic chemistry, and should not be undertaken lightly by amateurs." At the end of that volume, Richard C Hall HI presents a "DEA Watched List of Chemicals." Many of these substances arouse suspicion only if bought in large or repeated orders, but others "are suspect under any conditions."
A further complication, exposed in a March 1981 High Time; editorial ("LABSCAM") and an accompanying article ("Anatomy of a Sting"), has been the Drug Enforcement Administration's use of Buckeye Scientific, a Columbus, Ohio chemical supply firm, and other scientific companies to "suck unsuspecting would-be bathtub chemists into a trap that could imprison them for years." That "Buckeye and other DI:A snitches," High Times declared,
advertised their set-up scams. in High Times has brought an embarrassment the magazine will not soon live- down .... They recruit would-be chemists to buy raw materials, they deliver the Supplies themselves; they allow the carefully cultivated labs to pump out and sell batches of amphetamines, LSD, methaqualone and other bathtub concoctions Finally, they bust the labs—labs that virtually could not exist without their participation ....