We run single foram samples, normally 10-30 ug, on the Kiel IV + Thermo Delta V plus, with same size NBS19. Our long term precision is 0.05 for d13C and 0.10 for d18O, for small samples (size 10-30 ug). Even though I require sample size must be >10 ug to give reasonable delta values, sample size down to 8 ug also can yield enough gas for a reasonable analysis.


Wei Huang, Ph.D.

 

Stable Isotope Lab Manager


New Core Lab Rm#212

Lamont-Doherty Earth Observatory of Columbia University

61 Route 9W
Palisades, NY 10964
Lab:
845-365-8143
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On Wed, Oct 25, 2017 at 12:24 PM, Alan Mix CEOAS <[log in to unmask]> wrote:
MAT252, Kiel-III, capillaries balanced at low voltage, cleanliness is next to godliness, no slope corrections, “normal” glass reaction vials.  

Results to 10 micrograms on calcite standards — see graphic below (in the 10-21 microgram range, d13C external precision of 0.03 to 0.04, d18O external precision of 0.03 to 0.06 --two different numbers because two different standards, offset between standards maintained at about 5.5 permil for d18O, 1.2 permil for d13C, so no problem with gas mixing or memory).  Results on real biological samples will be less precise because of, well, biology.  

I’m not particularly fond of approaches that that do slope corrections as a function of mV as they can make standards look OK but you never really know they are right. Not religious about this, but very cautious. Can’t fight physics  — if the capillaries jump flow regime at low pressures, that’s the limit and the two sides don’t necessarily do it at exactly the same point.  On our current system, the practical limit appears to be about 10 micrograms.

Alan.



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Alan C. Mix, PhD
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Oregon State University
CEOAS Administration Building 104
Oregon State University
Corvallis, OR 97331-5503 USA

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www: http://ceoas.oregonstate.edu/profile/mix/



On Oct 25, 2017, at 7:30 AM, Christopher Maupin <[log in to unmask]> wrote:

Dear Isogeofolks, a broad, community query here: 

I’m curious what your successes and/or failures running extremely small carbonate samples have been like. Seeing the uptick in individual foram papers in recent years as piqued my curiosity to reach out to the broader iso-sphere. 

What instrument/peripherals have you tried/are you using?
What are the smallest masses of CaCO3 you are able to successfully measure?
What precision are you routinely achieving on these successful measurements? 
What is your “recipe” for success?

Many thanks!
________________________________________________
Chris Maupin, Ph.D.
http://christophermaupin.strikingly.com
Research Associate and Facilities Manager
Stable Isotope Geosciences Facility (SIGF)
Geography Department
Texas A&M University
405 Eller O&M Building 3147 TAMU
College Station, TX 77843 USA
Email: [log in to unmask][log in to unmask]
Mobile: (512) 810-8437