BRUKER D4 Endeavor XRD
- jr_barnes
- Former user (Deleted)
Nov 29, 2022 The D4 has been used for all measurements this expedition. Preventative maintenance was performed on the Haskris, so the instrument was shut down for less than a day.Â
Aug 24, 2022 PC Mover was used to transfer the Bruker folders and files from the old computer to the new XRDIH. During this process, however, approximately 30- 40 files were missing, mainly from the DIFFPLUS folder on the C drive. This rendered the D4 unable to analyze samples entered into the 'Jobs' tab of XRD Commander as the sample would be loaded, then immediately unloaded an error displayed. Samples could still be ran manually in the 'Adjust' tab, but this would not be tenable during an expedition. Once the files were restored, this issue was resolved.
Aug 17, 2022 The Bruker vendor visit was successful and the D4 is running smoothly again. The problem was diagnosed as a failing power supply in the rack. This was replaced with a new power supply unit. A new x-ray (SN: 543795) tube was also installed and the beam alignment adjusted. The old x-ray tube (SN:541660) that was installed in Sep 2019 was placed on the top shelf in the sample prep area of the Thin Section Lab. The x-ray tube that was removed in Sep 2019 will be sent back to College Station. The issue of the sample swing dropping samples was not addressed specifically, but all drives were checked and operating as expected and the technician was happy with their alignment. The cover above the sample swing can be removed if a sample needs retrieving from this area.
From the Bruker Service Report: 'General Service & Instrument Switching off. On arrival, instrument not booting up. Found CMOS battery flat - replaced battery. Set BIOS up and save. Shutter error - checked shutter - fine. did general service. removed dust and lubricated auto sampler. Checked belts - all fine. Checked all fans - working. Replaced X-ray tube. Did alignment and tested system with corundum std. All in spec. System switching off - faulty power supply - replaced. Test results: 25.576 → 25.572, diff 0.004, FWHM Obs: 0.072, 35.149 → 35.146, diff 0.003, FWHM Obs: 0.068, 88.994 → 88.985, diff 0.009, FWHM Obs: 0.094, 127.680 → 127.672, diff 0.008, FWHM Obs: 0.163. All data saved under C:DIFFDAT1 Cape Town 15/08/2022.'
Jun 13, 2022 The instrument was tried at the beginning of Exp 393, but would not stay on long enough to run even one sample. Therefore, the instrument was shut off on ?? for the duration of the expedition, as well as the Haskris.
A Service visit has been scheduled for 15-17 August during the tie-up Exp 397P in Cape Town.
Jun 6, 2022 Artifact peak at 7º 2θ is from the plastic backloading sample holders. Empty PMMA plastic sample holder was analyzed and the peak is identical. Ran two samples on each of the holders to compare, along with empty scans of each. This was added to the Exp390 X-Ray Technical Report.Â
Also, when starting up the Bruker, a fuse in the power cord blew twice. The ET replaced the fuse with one of higher amperage (4 Amp as opposed to 3 Amp). This should be conveyed to the service technician during the next site visit in Aug.
May 30, 2022 The current situation is that the X-ray tube, high voltage cable or detector is failing on the Bruker. A new tube has been ordered and should arrive in time for Exp 393, however, it will not be installed until Exp 397P by a Bruker service technician. This site visit is still being scheduled (approximately 10-17 Aug 2022 in Cape Town). The service technician will also do other checks to help ensure we can keep going with the D4. As the support technician pointed out, however, some components of the D4 are now obsolete (including the Vantec-1 detector).
The Bruker can still analyze samples, but it will shut off randomly. There is a sign posted on the Bruker about how to finish powering down the machine before it can be started back up. It has started back up again just fine 99% of the time. If it does not start back up normally, give it an hour and try again. If it turns off mid sample, upon restarting when you initialize the drives in XRD Commander, it should bring the sample(s) it was analyzing back to the positions they came from on the sample table. A few times the sample holder has been misaligned and the sample swing will stop. Retrieve the sample, restart XRD Commander and initialize the drives again. It should go again without issue. I think this is an alignment issue, but I am too inexperienced to mess with the sample handler at this point. Maybe Heather can assist with this issue? When starting to measure again, it can continue measuring the same sample as long as you use the same method program and enter the exact same file name for the sample in XRD Commander. After you select 'Start' when you've entered the jobs again, a window will pop up to ask if you want to continue. If you select 'Yes', it will finish the scan.
There is an artifact peak at 7º 2θ that now appears in all the powder scans (but not the corundum standard scans), I have contacted Bruker about this and discussions are ongoing about the cause of this peak. If this is a problem for the scientists, samples can be run on the Aeris.Â