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Standard Operating Procedure – X-Ray

March 2018 - v.375

Find your room and bunk assignment, drop your luggage off.
Go to your lab and begin cross over with the off going technicians.
Read the lab report from the previous Expedition and discuss any changes in equipment status or procedures. This can be found on Confluence XRD Lab Notebook.
Attend introductory meeting with all IODP staff or any other safety or training meetings.
Assist with loading/unloading of cores, freight and other tasks as directed by the Lab Officer (LO) or Assistant Lab Officer (ALO).
Unpack all oncoming freight and distribute them accordingly
Verify physical counts on priority #1 inventory items for XRD, ICP Prep, and pXRF. Bring to LO/ALO's immediate attention if any item is short on quantity.
Read the XRD manuals for instruments you will be using.
Collect and remove all trash from your lab before sailing. There will be a trash container not he dock side, ask ALOs for confirmation.

Check water level and temperature of Haskris chiller. Ensure filter is clean.
Before running the Bruker D4, initialize the sample changer from XRD Commander Program or if from a complete shutdown initialize sample changer first using D4 tools, then initialize using Commander, then run 'tube conditioning program in D4 Tools. (Instructions are in the XRD Bruker Manual).
Run QAQC Standard in Bruker D4 as detailed in manual.
Coordinate a work area in the fume hood with the chem tech and make sure there is a 10% Nitric bath available for cleaning quartz and platinum crucibles.
Familiarize yourself with the expedition prospectus and ascertain a likely number of ICP, XRD, and pXRF samples that can be processed. Discuss sampling with Curator and applicable scientists. The core lab is your primary duty and x-ray must come secondary to that unless arrangements are made with the Lab Officer to meet specific objectives. Scientists should be made aware of this and that it is not reasonable to expect high resolution on a high recovery expedition.
Provide training to scientists on using XRD software (EVA and Highscore)
Provide training to scientists on hand held XRF in instrument operation, sample preparation, and data upload/download procedure
Provide XRF safety training to scientists who uses hand held XRF. Check out and assign dosimeter ring to individual scientist. Ensure they understand all safety concern and sign required document.

Primary duties are assisting as needed in the core lab and on the Core receiving platform. For details on Core lab responsibilities refer to the Core lab SOP.
Prepare XRD, ICP, and pXRF samples for analysis.
Read available literature to understand the theory and operation of XRD, ICP, and pXRF analysis. Be prepared to answer questions or at least point a scientist or tech in the right direction.
Keep X-ray lab and ICP prep area clean. A high level of cleanliness must be maintained at all times during ICP preparation. Frequent vacuuming will keep dust to a minimum.
Maintain a chronological log of lab events to assist in an accurate Technical report at the end of the expedition.

Save Bruker XRD files in *. raw, *.pdf or *.png and *.uxd format. Upload the XRD files to LIMS.
Save Aeris XRD files ??? (Aeris file saving is being discussed by Lab Working Group)
Save pXRF files in *.csv and *.spm files. Upload XRF files to LIMS.
Verify that all samples have been analyzed by running a LIMS Report query.
Upload LOI Spreadsheet to LIMS.

Maintain AMS inventory sheet. Do physical counts of supplies.
If the equipment is not operating properly, learn how to fix it. Only qualified technicians should attempt to make more than minor adjustments or repairs to the instruments. The Xray technician should attend the Bruker, Olympus and Aeris courses if available on shore to become qualified at identifying problems and trouble shooting. Communicate with vendor technicians (Bruker, Olympus Aeris) and E.T's if assistance is required.
Monitor oil levels in vacuum pumps. Change oil regularly, and perform one full service and maintenance of pumps per expedition.
Monitor water level in Haskris water pump. Clean or change water filter as necessary.
Ensure desiccant in desiccators is dry and ready for use. Oven dry if necessary.
Clean freeze-drier valves, vials, and the desiccators. Replace filters as required. Drain water from the unit and dry inside. This is performed as needed (~ once a week).
Record and date any maintenance in the XRD maintenance log on confluence. For all correspondence with vendors, ALO and LO's concerning maintenance and repairs, CC your cross shift.

Receive core and assist as needed in the core lab (i.e. splitting, restocking, boxing core, disposing of trash, and general cleaning and maintenance of core lab). Remember, the core lab is your primary duty and XRD/ICP preparation must come secondary to that unless arrangements are made with the Lab Officer to meet special objectives.
Maintain inventory by checking quantities and performing physical counts. Notify the ALOs if any quantity discrepancy or unusual high usage occurred.

Write the end-of-Expedition tech report, follow the outline of the previous report, give a copy to the Lab Officer.
Make sure all data are sent to LIMS before the MCSs cut off database access. All non-essential data should be erased from the hard disks of all the computers.
Work with the Curator and scientists to determine where residue powders will be sent.
Pack up equipment being returned for repairs and give the Assistant Lab Officer the following information: IODP inventory number, value, weight, serial number, model number, vendor's name and country of manufacture.
Give the Lab Officer a list for port purchases if any.
Clean the lab and assigned area following the cleaning instruction listed by the LO/ALO. Bring all the trash to the incinerator. Glass and sharps get disposed of in port call.