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Ahoy,

I have myself encountered this problem and do not fully understand why it sometimes occurs but not always and not for everyone. But it is most certainly the result of Oxygen/oxidation. Aside from the usual recommendations which you seem to have already adhered to I can at this point only recommend to find the means to perform your synthesis under inert gas. Or alternatively, to employ a coating/capping agent such as Oleic acid.

There are a number of publications easily found which use Oleic acid (OA). While we do not have a proper protocol for you at this point I can tell you that the addition of OA, post initial Fe solution precipitation, while otherwise sticking to our protocol should work and may solve your issue.

I will talk to my colleagues and see whether they have some further recommendations.

Best regards

Tim

 

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