Microanalytical Chemistry: Protocols for preparing low-volume calibration standards

Chemistry Asked by M. Farooq on July 27, 2020

Does anyone have an example of a protocol for preparing very small volumes (about 1 mL) of highly reliable analytical standards in organic solvents such as ACN, MeOH, and DCM etc in part per million range (~ 1- 2000). The reason to use small volumes is the limited amount of analytes. More specifically, I am looking for an example as to how NIST or other certified reference material providers prepare standards of compounds in organic solvents. If we have a solid analyte in milligram amounts, what would be an accurate way of preparing standards? Similarly, if we have a liquid analyte, what would be the best protocol for volume transfer.

BTW, I am surprised by the inaccuracy and imprecision of mechanical micro pipettes for transferring volatile organic liquids. Even the angle of holding the pipettes and the time of holding the pipette in the liquid changes the delivered volumes. So this option is out.


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