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34 S Analysis of Solids by EA-IRMS
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Sample Preparation Material needs to be dry and homogenous Organisms can be analyzed whole if small enough Sample weights: 20-30 µg sulfur < 20 µg sulfur by arrangement Most organic samples are 0.1-1% sulfur dry weight
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Encapsulating Samples Weigh samples into tin capsules Add oxidant: 2mg of V 2 O 5 or No 2 O 5 to each capsule
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Organizing Trays Load samples across rows of 96-wells trays Do not leave empty wells between samples Label trays uniquely and clearly Place samples for different analyses in different trays
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Paperwork Complete an Analysis Order Form for each analysis type Complete a sample list for each Analysis Order From Email forms to sif@ucdavis.edu Include printed copies with samples
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IRMS Methodology 32/34 obtained from measurement of SO 2 ion beams, 64/66. Modification of Baublys et al. 2004. Baublys, K., Golding S., Young, E., & B. Kamber. 2004. Rapid Commun. Mass Spectrom.
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The SO 2 problem: Oxygen Isotopes Oxygen isotopes will produce bias in measured 64/66 ratios Solution(s): measure or minimize variation in oxygen isotopes 64 SO 2 32 S 16 O 16 O 66 SO 2 34 S 16 O 16 O 33 S 17 O 16 O 32 S 17 O 17 O 32 S 16 O 18 O Relevant isotopomers of SO 2
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Oxygen Homogenization Oxidant and molecular oxygen used in flash combustion supply reservoir of donor oxygen during SO 2 formation Hot quartz chips further homogenize oxygen signal
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Chromatography
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Sulfur Data Reduction and Corrections Blank Drift Size Scale expansion Corrections follow those of Kaiser and Röckmann 2008 Kaiser, J. & T. Röckmann 2008. Rapid Commun. Mass Spectrom.
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