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I am NOT soliciting information on how to procure illicit substances... but I am idly curious how rationalists are getting precisely dosed psychedelics

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Synthesizing the psychedelics themselves, or having a chemist they know do it. TiHKAL was the classic reference on this.

Dark-web sales and purity testing labs? That meshes with the techno-libertarian side of things, but I have no idea how those labs operate and I'm guessing buying drugs online practically requires you to commit a federal crime in the US, which is a pretty big hazard.

For many of the psychedelics active in the μg range, cheap affordable lab tests (low end spectroscopy) will not be sufficient to even detect the compounds of interest. They would just say that the drug is on blotter paper, for example. Expensive analysis defies the point, and it also much more closely monitored, unless you have a friend at a university research center.

Many psychedelics have unclear scheduling around the world, and can be "legally" sold "NOT FOR HUMAN CONSUMPTION". The US has the Federal Analogue Act that catches a lot of the {1V,1P,1cP,1D}-LSD prodrugs that need to be explicitly scheduled in many other countries. So for LSD (or LSD prodrugs), in the US, I will guess that people with genuinely accurate information on doses are synthesizing it themselves. This carries much higher penalties than simple possession and could be construed as manufacturing or possession with intent to distribute. I personally would not risk the ire of the famously fickle US govermental agencies just to a slightly more accurate read on the dosage of drugs.

Addenddum: Alexander Shulgin, the author of TiHKAL, obtained a DEA Schedule I license to perform his experiments.

In 1994, two years after the publication of PIHKAL, the DEA raided his lab. The agency requested that Shulgin turn over his license for violating the license's terms, and he was fined $25,000 for possession of anonymous samples sent to him for quality testing.

So people do go indeed go around shipping samples to chemists in the US for testing, though I'm guessing for purity/lack of contaminants, not concentration.

Laws are shifting fast though, and I'd expect within a decade, you might be able, under clinical contexts, to access certain psychedelics.