Frustrating monochromator glitch
Dear mailing list - my last round of EXAFS experiments performed on the Fe-K edge in fluorescence mode gave data extending nicely to 15 in k. One problem was a nasty monochromator glitch at approx 13.5 in k which is so great in some cases it causes sufficient distortion to the data that even upon deglitching I must cut back the data to 13 in order to gain a good fit using my models. Firstly I was wondering if someone here could describe to me how a monochromator glitch arises (some systematic defect in the monochromator crystal or more? - the only problem with this explanation is that some data sets seem more affected than others and it has not manifested itself as badly in previous trips). Also is there any other way to handle the removal of a monochromator glitch besides deglitching? My supervisor seems to think that there must be a scale factor or offset in the I0 monitor counts which could be corrected in order to overcome a glitch in the existing data - has anyone ever ! thought of other ways to salvage data in this way? Regards, Mark -- Mark Bondin PhD student School of Chemistry, University of Melbourne (03) 8344 7015 (Tower lab) 0409 252 983 (mobile)
Dear Mark: A monochromator glitch is when, because of some small misalignment of one of the two (generally) monochromator crystals, a parasitic reflection comes into Bragg alignment and reflects a significant maount of intensity off into a direction which is not towards the sample. These reflections can be shifted around or removed by tweaking the crystal in question in one of the two axes perpendicular to the primary axis of rotation of the monochromator. Sometimes this is not possible (as with a cryogenically cooled first crystal where these additional motions are not readily available) and you just have to live with them. You will notice the Io drops precipitously at a glitch and this will cause a reduction of intensity in your It or If detector as well. If the detectors which you are using are well matched in their response to changes in intensity, the glitch is mitigated in the ratioed XAFS data. This is usually possible to do in a transmission experiment, where both detectors are ionization chambers. You can test for this before starting your data collection by plotting the ratio of Io/It and deliberately attenuate the beam. If the ratio remains constant, you have a good chance of not seeing the effects of the glitch in the data. It is much more difficult when you are doing fluorescence experiments since the fluorescence detector is hardly ever a perfect match with Io. In these cases, you just have to try to minimize the differences in response by trying different things. With a Fluorescence Ion chamber, you might try increasing the potential on the chamber (just as long as you don't get a shock!). With a solid state detector, you just have to fuss around until you are satisfied that you have the best match between detector responses. There is no way that I know of correcting numerically for nonlinearities in the two detectors. Deglitching will have to be done. In fact, you need to make sure that the nonlinearities are not effect on the shape of the edge itself, since that is potentailly a place where there is a significant change in intensity in one of the detectors. I am sure that I haven't covered everything. Hope this helps, Carlo On Thu, 9 Dec 2004 m.bondin@pgrad.unimelb.edu.au wrote:
Dear mailing list - my last round of EXAFS experiments performed on the Fe-K edge in fluorescence mode gave data extending nicely to 15 in k. One problem was a nasty monochromator glitch at approx 13.5 in k which is so great in some cases it causes sufficient distortion to the data that even upon deglitching I must cut back the data to 13 in order to gain a good fit using my models. Firstly I was wondering if someone here could describe to me how a monochromator glitch arises (some systematic defect in the monochromator crystal or more? - the only problem with this explanation is that some data sets seem more affected than others and it has not manifested itself as badly in previous trips). Also is there any other way to handle the removal of a monochromator glitch besides deglitching? My supervisor seems to think that there must be a scale factor or offset in the I0 monitor counts which could be corrected in order to overcome a glitch in the existing data - has anyone ever ! thought of other ways to salvage data in this way?
Regards,
Mark
-- Carlo U. Segre -- Professor of Physics Associate Dean for Special Projects, Graduate College Illinois Institute of Technology Voice: 312.567.3498 Fax: 312.567.3494 Carlo.Segre@iit.edu http://www.iit.edu/~segre
Hi Mark,
Dear mailing list - my last round of EXAFS experiments performed on the Fe-K edge in fluorescence mode gave data extending nicely to 15 in k. One problem was a nasty monochromator glitch at approx 13.5 in k which is so great in some cases it causes sufficient distortion to the data that even upon deglitching I must cut back the data to 13 in order to gain a good fit using my models. Firstly I was wondering if someone here could describe to me how a monochromator glitch arises (some systematic defect in the monochromator crystal or more? - the only problem with this explanation is that some data sets seem more affected than others and it has not manifested itself as badly in previous trips). Also is there any other way to handle the removal of a monochromator glitch besides deglitching? My supervisor seems to think that there must be a scale factor or offset in the I0 monitor counts which could be corrected in order to overcome a glitch in the existing data - has anyone ever ! thought of other ways to salvage data in this way?
The convential mono glitch comes about when another Bragg reflection from the monochromator becomes allowed. For example, with a Si(111) mono, you can get to an angle where a higher order non-harmonic reflection is in the diffraction condition -- say, a (311) or (220) or (11 7 7) reflection. The presence of these reflections robs intensity from the main reflection, giving less intensity at that energy. Glitches seem to come in groups of 2 or 3 (sometimes 4), which probably corresponds to just grazing throught the Ewald sphere of a family of reflections with same nominal q. Glitches can come from either the first or second crystal of a double crystal monochromator. Ideally, you'd like to be able to rotate the crystals azimuthally -- I don't know of any beamlines where this is under the user's control!! But there are a few thing you can try to reduce the impact of glitches. First, try changing the detuning of the 2nd crystal to one side and then the other of the rocking curve. It might move the glitches, or it might do nothing. Next, try moving both the first and second crystal with whatever other motions you have. Again, this might do nothing, but you might get lucky. Third, find out about how 'feedback' is done, and play with this. Sometimes, you can stabilize the intensity this way, minimizing the impact of the glitch. But before you start messing around with the mono, a loss in I0 intensity is supposed to normalize out of EXAFS, so question why it does not rather than blame the glitch for screwing up your data. Here are some questions to ask when glitches don't normalize away: Are the harmonics really being rejected ? Are the ion chambers really working in a linear regime with flat voltage-intensity curves? Are the dark currents measured and being subtracted correctly? Is the beam being clipped somewhere or is incompletely defined by slits and any mirrors? How uniform is the sample? Hope that helps, --Matt
participants (3)
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Carlo U. Segre
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m.bondin@pgrad.unimelb.edu.au
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Matt Newville