Standard Operating Procedure - Chemistry Lab
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- Do a thorough cross-over with off-going Chemistry Technicians : read Tech Report, discuss every instrument separately and bring to the attention of the ALO/LO any equipment requiring immediate attention.
- Unpack new supplies and store in their correct location. Remember to mark on the bag/container the current Expedition number.
- Conduct an inventory of chemicals in the storage cabinets. Look for any chemicals not on our inventory, unmarked containers, or reagents or mixtures left over from the previous expedition. Bring any issues to the attention of the LO.
- You should calibrate as many instruments as you can. Instructions are in the instrument-specific User Guides. Make as many reagents as you can.
III. SITE PREPARATION - Prior to arrival on site and core-on-deck
On cruises with short transit times, perform as many of these as possible in port.
Lab orientation/Introduction
- Give an orientation/safety procedures tour of the lab to the Chemists.
- Meet with Chemists and find out their general goals and specific requests. If there are Microbiologists sailing make sure that these same protocols are done with them.
- Divide up responsibilities among the Chemists for all shipboard analyses.
- Have a meeting with the Chemists/Curator/EPM SAC (Sample Allocation Committee) to go through sample plans.
- Prepare sampling equipment and sample storage containers. Wash any necessary containers and prepare spikes if needed.
- Prepare SampleMaster split template (water and cake splits).
- Explain Show how to print sample labels.
- Go over any and all MSDS sheets before working with any chemicals. Understand the risk of handling chemicals, especially if any hazardous chemicals will be used.
- Print out the most recent copy of each instrument's User Guide so the Scientists can become familiar with each instrument's operation.
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Check the pressure of the oxygen (ChemLab), helium and argon bottles (Tween Pallet Stores). Ensure the bottles are above 200psi200 psi; otherwise, swap them out with fresh bottles.
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IAPSO - Store it properly, as any evaporation will lead to increased salinity.
Necessary IW squeezing supplies:
- 50mL 25/50 mL plastic syringes (acid-washed).
- 0.45µm Whatman disk filters.
- Take four boxes of 9 cm #1 Whatman filters and soak them in a large beaker of DI water for ~2hours, then oven-dry at a low temperature (~50oC). When they are dry, store them in Ziploc bags near the Carver presses. You may need to do this again during the Expedition.
- Obtain necessary containers for IW sample splits. At the Scientist's request they may need to be rinsed with DI water/acid washed and dried. Also prepare necessary sample spikes.
- Bags for squeeze cake splits and baked aluminum foil (if required bake at 500 C for 8 hours).
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- Headspace sampling tools and containers (vials, septa, crimper).
- Gas void assemblies (50mL 50 mL syringe and three-way stopcock, with male luer lock, attached to the core liner puncturing tool).
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- 10% HCl bath for general glass/plastic ware plasticware cleaning. 10% HNO3 3 bath for ICP
- Paper towels
- Kimwipes
- Pipette tips
- P-boxes (for sample storage; foam ampule holders for glass vial storage)
- Gloves, various sizes
- Boxes for cryovials
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- Take a 5 cc headspace sample from every sediment core (non-basement), at the top of a section (try to be consistent). This sample is taken until the total depth objective is met. If doing multiple holes, you do not have to repeat the sampling if the sample is taken at a prior depth but just continue after the prior hole's bottom depth.
- For cores with IW samples, take the headspace sample from the top of the section immediately below the IW sample. Note the core, section and interval of the headspace sample and write it on the Curator's logsheet. The interval will need to be entered into SampleMaster by the Curator/ALO.
- Make sure nobody sprays acetone on the catwalk before sampling is completed. Acetone will contaminate the sample.
- It is recommended to occasionally take a sample of the air on the core deck, so that any change in the headspace sample analysis can be correlated to changes in volatilized acetone.
- Inject a standard (corresponding to a similar concentration seen in the core samples) every fifty injections or so, to check on the instrument calibration.
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- Set the pressure gauge around 3000psi and simultaneously push and hold both green (CLOSE) buttons on the hydraulic unit's base until the auto-pressure engages.
- After the first drops flow from the hole in the squeezer's base plate, insert the syringe into the hole. Keep an eye on the syringe to make sure the pressure doesn't push out the syringe or plunger (especially for the first few cores). Keep incrementing the pump pressure in sets of 2000lb. Do not ever increase the pressure above 30,000lbs.
- Select the correct core, section, and sample, and upload the IW sample splits (using the Excel template) into SampleMaster and distribute the labels.When porewater yield is sufficient/no more water is trickling, release the pump by pressing the red OPEN button and remove the syringe from the squeezer.
- Start sample distribution (splits).
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- Fill the Carver presses with oil (if necessary).
- Check the oil in the freeze dryer's vacuum pump.
- Defrost and clean the freeze dryer.
- Clean (defrost if necessary) the fridges; dispose of old reagents.
- Change the hydrogen generator's DI bags and vacuum the back vent filters.
- Check the ovens for debris.
- Clean any instrument-specific items.
- Have the lab coats laundered (segregated and tumble dried).
- Immaculately clean the lab (this means everything).
- Check expiration dates on chemicals, notify ALO/LO if hazardous chemicals/waste need to be disposed in port.
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