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Laboratory

Solid - δ13C, δ15N

Overview

We use a Costech Elemental Analyzer, Conflo III, MAT253 for a continuous flow based measurement of our solid organic material δ13C and δ15N. Samples are flash combusted at 1000 °C with excess oxygen in a Costech ECS 4010 Elemental Analyzer (EA) equipped with a zero-blank autosampler. The combustion column was packed with cobaltous oxide for a combustion aid and silvered cobaltous oxide to scrub sulfur compounds. A helium carrier set to 80 mL / min moves combustion products through a 700 °C reduced copper column to ensure complete reduction of NOx compounds to N2 and also to absorb all excess oxygen. Sample gases were then carried through a magnesium perchlorate trap to absorb all water and then through a 3 m gas chromatography column to separate N2 from CO2. The EA effluent flows into a ThermoFinnigan Conflo III where the stream is split to reduce the flow rate from 80 mL / min to 2 mL / min. The reduced flow rate then flows through an open split with excess helium via fused silica capillary tubing. A pressure differential between the ThermoFinnigan MAT253 isotope ratio mass spectrometer and the Conflo III along fused silica capillary tubing allows helium and sample gas to move into the electron bombardment source for subsequent ionization, acceleration, focusing, separation, and measurement of masses 28, 29 for δ15N and 44, 45, 46 for δ13C. Internal laboratory reference materials are interspersed with samples for a two point calibration which allows for blank correction and conversion to the δ15N Air-N2 and the δ13C VPDB scales. We have an assortment of in-house standards calibrated against the international reference materials NBS19, LSVEC, IAEA-N-1, USGS32, USGS40, and USGS41.

The IsoDat software provided δ15N and δ13C values relative to the respective reference gas cylinders (along with all other selected data) are imported into a matlab script for data reduction. A linear regression is completed, independently for δ15N and δ13C, using the measured δ values and the accepted values of our internal reference materials. All data are corrected to the Air-N2 scale, for δ15N, and to the VPDB scale, for δ13C using these respective linear equations. Precision and accuracy are estimated for each run using a third internal reference material that is treated as an unknown. Reference materials are chosen to bracket the sample range in δ15N and δ13C values.

Sample submission

If you are interested in both nitrogen and carbon isotope data, provide enough material such that 40 µg of nitrogen and 200 µg of carbon are consumed per analysis. If you are interested in carbon only, provide enough material such that 20 µg of carbon are consumed per analysis. We recommend loading samples in either 5x9 mm or 3.5x5 mm tin capsules and using a standard 96 well plate to transport them. You need to know the approximate percent nitrogen and percent carbon of your samples so that you or we know how much material to load into each tin. For example, our salmon standard is about 11.8 % nitrogen. Ideally, each tin will have 339 µg of this salmon standard loaded (40 µg N / (11.8 % N / 100) = 339 µg N). If samples have unknown quantities of nitrogen or carbon, you will likely need to run test samples of your material for content analysis. Preparation and analysis costs are here. This method requires at least Solid Sample - δ13C and δ15N for isotopic abundance measurement and may also require Lyophilize, freeze dry, Sample Acidification , Simple sample grinding , and Sample Loading.

Standard Operating Procedures

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