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I have an intercalated layered crystal whose composition I want to determine in particlular the amount of intercaltion. Since single crystal xrd may be difficult, I was advised to try powder x-ray.

Is there a recommended powder x-ray method for intercalated layered crystals? For instance, I tried to no avail extended ultrasonic shaking in acetone to powderize the crystal but it didn't work. Also, wouldn't grinding a layered crystal affect its xrd pattern?

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    $\begingroup$ If the sample is already a single crystal, then the only way I know of making it into a powder is grinding it. If you're concerned about mechanical stresses somehow introducing defects into the powder crystallites which might affect the powder x-ray diffraction pattern, you could try first cleaving the single crystal into two or more pieces so you don't grind up all of the single crystal at once and can try alternative grinding methods. $\endgroup$ – Samuel Weir Feb 19 '17 at 4:59
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    $\begingroup$ you should better spell out xrd = X-ray diffraction. $\endgroup$ – wonderich Feb 19 '17 at 17:51

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