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Chemical Stability and Compatibility - Stability of Ta and Nb upon dilution

 
Hi-I'm having trouble with diluting a custom standard, and I believe that your preparation is fine- I just can't get the elements calibrated by ICPMS. Most of the elements (V,Ce, Hf, Nb, Th, Y, Yb, & Zr) calibrate just fine. Unfortunately, I can't get successive dilutions of the standard to give linear calibrations for Ta & Nb, regardless of repeated preparation, the isotope monitored, or immediate use of freshly prepared standards. Since your company has mastered keeping these elements in solution, could you offer some advice as to how to keep the Ta & Nb "well behaved" while using your standard? Would a complexing agent help? I've been using 2% nitric; while your standard is in 5% nitric + trace HF. Could I get away with using 5% nitric without the trace HF and expect good behavior?Any advice you could offer would help.
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Depending upon the final diluted concentrations it is possible that 2% HNO3 only is not capable of stabilizing the Nb and Ta. We have observed low ppb levels of Ta are not stable long term (e.g., weeks) when diluted solely in 2% (v/v) HNO3, and we would recommend increasing the HNO3 content to 5% as it could help with this issue. If that does not solve the problem, then adding trace HF (0.1% v/v or less) would likely solve the issue. It is also possible that aggressively cleaning the preparation containers could help stabilize the diluted standards, as we have observed that <100 ppb mixed element solutions often benefit from storage in pre-cleaned containers. In that regard, our recommendation would be to leach the labware in 5% (v/v) HNO3 at 60 degrees Celcius for at least 60 hours followed by extensive rinsing. It may be that a combination of higher HNO3 content (5% vs. 2%) in conjunction with acid-leached preparation containers would solve the issue, at least to the extent of allowing daily measurements to proceed.

Posted: 09/02/18 21:56:42

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