PROTOCOL FOR PREPARING SUPERSATURATED PHOSPHORIC ACID FOR CARBONATE ANALYSES

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Introduction

The following protocol describes the analysis of carbonate samples for δ13C and δ18O at a Kiel IV carbonate device.

Safety info


Wear cryo-gloves, long sleeve shirts, protection glasses and closed shoes when handling with liquid nitrogen in open dewars. Liquid nitrogen is an extremely cold material. The vapor of liquid nitrogen can rapidly freeze skin tissue and eye fluid, resulting in cold burns, frostbite, and permanent eye damage even by brief exposure.


In the event of spillage of liquid nitrogen on a person If exposed to liquid or cold gas, restore tissue to normal body temperature, 37°C, followed by protection of the injured tissue from further damage and infection. Remove or loosen clothing that may constrict blood circulation to the frozen area. Rapid warming of the affected part is best achieved by using water at 42°C. Water should under no circumstances be over 44°C, nor should the frozen part be rubbed either before or after rewarming. If in doubt contact Legevakt (phone 116 117 or 113 for emergencies).

If someone get liquid nitrogen it in the eyes, call 113, wash the eyes with appropriate equipment immediately.

Sample identification


A sample list should first be made: total amount of samples, Sample ID (from user), type of material, Lab ID (project no) ect. The analyses project must be registered in the project database http://delta.geo.uib.no:8085


Weighing in standards/sample material

Equipment: Spatula, tweezers, tray, brush, weighing boat, paper box for vials and clean Kiel vials.

  1. Write yourself on the list/check if the microscale is available.
  2. Clean the working bench and other weighing equipment with Kim Wips/brush.
  3. Do not place vials, racks or other equipment on the anti-vibration table or on top of the microscale to prevent destabilizing the balance.
  4. Use a 253-run sequence sheet for plotting information needed (Sample ID, Project no, sample material ect.
  5. Find CM12 and NBS18 in the standard desiccator.
  6. Open the standard bottle only when you take out standard and close it immediately after use. DO NOT PUT MATERIAL BACK INTO THE STANDARD BOTTLE AND NEVER POUR STANDARD OUT!
  7. Weigh in between 30 – 70 μg of the material.
  8. Carefully lead the boat towards the microscale by using a tweezer.
  • If the weight is too large: remove the boat from the microscale and pick/pour the extra grains out on the tray/weighing paper. You can reuse standard material if the trey/paper is clean.
  1. Clean the top of the vials with your fingertip and before you carefully lead the boat towards the bottom of the vial in a horizontal position.
  2. Clean the top of the vials with your fingertip before you carefully lead the boat towards the bottom of the vial in a horizontal position.
  3. Turn the vial and boat in a vertical position before pouring and carefully knocking the boat towards the wall to ensure that all material are located in the vial.
  4. Weight the empty boat again to double-check that it is no material left in the boat.
  5. Tap the vial with a tweezer to make sure all sample material is located at the bottom of the vial.
      Vial 1/1 and 1/2 (pump vials) must be clean and empty because these vials are not used for sample measurement. Placed the vial in the right position in the paper box.
  1. Repeat procedure from step 7.
  2. When changing to a new standard /sample use a brush and Kim Wips to clean all apparatus thoroughly to avoid contamination of standard.
  3. Place the standard back in the desiccator as soon as you are finish.
  4. If you leave the weighing room over time, make sure to cover all vials with a paper sheet to prevent dust and other impurities to fall into the vials.
  5. Once you are done, clean after yourself.


Running samples on 253

  1. Record date, filename, sample no, quantity of standards, ect in the logbook.
  2. Open Isodat 3.0 (if not already open)
  3. Click on double arrow symbol “>>” on the right-hand side of the taskbar to get an overview of the different Isodat modules/ programs (Fig. 1).
  4. An accessories bar appears on the left-hand side of the window: click on the pop out bottom (Fig. 2) on the “Dual Inlet” panel to open the Dual inlet window.
  5. Write down values/information in the blue logbook
    1. Dato, analyse nummer, antall prøver, antall std, filnavn ect.
    2. Vac and HV (visible in the MS panel on the left-hand side, figure 1) when the changeover valves are closed.
    3. Open changeover valves and perform a background scan to check the signal in the reference gas:
    4. Adjusting the bellow on the right-hand side in the Dual inlet window to approximate 10 and note the voltage at cup mass 44 (MS panel).
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