Stern-Gerlach experiment
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Originally done with (neutral) silver atoms in 1921, but even clearer theoretically was the hydrogen reproduction in 1927 by T. E. Phipps and J. B. Taylor.
The hydrogen experiment was apparently harder to do and the result is less visible, TODO why: physics.stackexchange.com/questions/33021/why-silver-atoms-were-used-in-stern-gerlach-experiment