Question
Asked 24th Sep, 2021

How do I calibrate the humidity chamber for moisture-dependent XRPD analysis?

Hi all,
I found our group has an "old" XRPD humidity chamber connected to some moisture-control system. The moisture-control system has a sensor that detects the humidity of the air it sends to the chamber, but we would like to be able to check the humidity in the chamber as well to be sure at which RH we run our XRPD.
Does any of you know if/how this is usually done? Is there a reference substance that one can use?
Thanks in advance for your help!
/V

Most recent answer

Wagner Da Nova Mussel
Federal University of Minas Gerais
Dear Valentina,
For sure it is not easy the way you want to do it. Usually, the internal measurement is done by the air resistivity between sensors, which changes with humidity a sort of conductivity pairs, similar to thermal pairs. In principle, you intend to check the information. The sensor calibration is physical, externally performed by the the pair resistivity. Best regards, WNM

All Answers (4)

Wagner Da Nova Mussel
Federal University of Minas Gerais
there are some digital humidity indicators that can be used, once previously calibrated.
Nevertheless, some chemicals may indicate the relative amount of humidity, in a relative precise way. Their use are conditioned to a well thermal treatment before use. It is somehow tricky.
Relative humidity cards indicators are widely used, check the link bellow:
Best regards,
WNM
2 Recommendations
Nobuyoshi Koga
Hiroshima University
I am using Humidity controller to introduce N2-H2O mixed gas characterized by different water vapor pressure into simultaneous TG-DTA and high temperature XRD instruments. In both cases, the gas generated by the humidity controller is transferred to an anterior chamber placed just before the gas inlet of the heating chambers through temperature controlled transfer tube. The anterior and heating chambers are also warmed by circulating hot water at a temperature higher 20degC than the dew point of the N2-H2O mixed gas. The temperature and relative humidity of the gas are recorded at the anterior chamber during the measurements of TG-DTA and high temperature XRD using a hygrometer. The water vapor pressure calculated from the temperature and relative humidity data is used as the actual water vapor pressure (kPa) in the reaction (heating) chamber.
I would be glad if this information is useful for You.
Best,
Valentina Leandri
KTH Royal Institute of Technology
Dear Wagner,
a humidity chamber for XRPD is made is very small and there is no space to fit a hygrometer inside (if it was so easy, I would not have posted this question here). The use of paper which changes color with humidity is also not possible: we need to monitor the relative humidity precisely and the chamber is made of metal, so there would be no way of seeing the paper from the outside while running an analysis. It is not a common chamber we are talking about, it is one for XRPD analysis (see attached picture). In any case, thank you for your suggestions.
Wagner Da Nova Mussel
Federal University of Minas Gerais
Dear Valentina,
For sure it is not easy the way you want to do it. Usually, the internal measurement is done by the air resistivity between sensors, which changes with humidity a sort of conductivity pairs, similar to thermal pairs. In principle, you intend to check the information. The sensor calibration is physical, externally performed by the the pair resistivity. Best regards, WNM

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XRPD Quantification - Building a calibration curve of drug excipient?
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  • Deleted profile
I am aiming to utilise XRPD to quantify a drug excipient within a drug product and have been having a little trouble building the calibration curve to allow for this quantification up until this point.
The calibration curve will have a y-axis consisting of the relative peak area of the excipient I'm hoping to quantify and the API (active pharmaceutical ingredient) which has a known concentration in the drug, and the % of excipient across the x-axis. I have already identified a unique peak for the excipient of interest to allow for peak area measurement. In terms of sample prep for the curve: I've prepared 8 samples which vary in the w% of the excipient, increasing at 1% intervals with each sample (18-25%) and the remainder being the API. I have run these on the XRPD, measured relative peak area but the resulting calibration curve is not what I expected.
Now, this is my main issue: I believe the issue is in sample prep. I have been told that the quantity of the API should remain constant across all 8 samples (although, I don't understand the logic of this if I'm measuring relative peak area?) and if this is the case then the total mass of the excipient/API mixture will vary across all 8 mixtures (to accommodate the increased excipient quantity) , with the sample holder then loaded for XRPD analysis.
If anyone with more experience with XRPD/calibration curves would care to point out anywhere I'm going wrong, or would care to explain why it's necessary that the API content is kept constant across all 8 mixtures of the calibration curve?
Any help would be greatly appreciated!

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