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One of the issues I have run into when using benzoate for the standards is that it does not contain any nitrogen. I am using a Thermo TCEA so the first peak I get when running leaves is N2 (28, 29). This tails badly and I am never convinced that it separates 100% from the CO. So as the column efficiency decreases with time a little more of it seeps into the CO peak. The only solution I have to this is to bake out the column after every run to restore the column to peak efficiency. I have been toying with the idea of making two benzoate house standards, determining their values using IAEA601 and 602 standards, then adding a small amount of imidizole to mimic the nitrogen in leaves. This way my standard would have the same amount of carryover from the nitrogen as the samples.

Todd Brown
Monsanto
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-----Original Message-----
From: Stable Isotope Geochemistry [mailto:[log in to unmask]] On Behalf Of Wolfram Meier-Augenstein (aps)
Sent: Wednesday, October 08, 2014 4:57 AM
To: [log in to unmask]
Subject: Re: [ISOGEOCHEM] Oxigen measurments in leaves and wood cellulose

Dear Jose,

In line with a previous response to your question I can only stress the importance of using the two benzoate reference materials (IAEA-601 and IAEA-602) as organic scale anchors to normalize your d18O values to the VSMOW scale.  You could also consider using reference waters (VSMOW, GISP, SLAP2) enclosed in silver tubes as available from USGS Reston's Stable Isotope Lab.

http://isotopes.usgs.gov/lab/referencematerials.html

With regards to matrix matched QC materials, you could use IAEA-CH-3 cellulose and monitor its longitudinal d18O value.  However, given the questions regarding its homogeneity, you could equally follow advice already given and purchase pure cellulose from e.g. Sigma-Aldrich (they do an "acid washed, from spruce" cellulose for column chromatography, which should be fine clean and homogeneous).

Two more matters that I consider important are (a) make sure your samples are dry and (b) make sure your samples stay dry.

(A) Instead of monitoring your lab's humidity level (and its isotopic composition), keep your 18O samples, QC standards and reference materials away from moisture / humidity by storing them in a desiccator together with a strong drying agent (phosphorous pentoxide).

(B) To keep your 18O samples, QC standards and reference materials away from moisture / humidity while sitting in the autosampler waiting their turn to be analysed, use a Costech Zero-Blank autosampler since this autosampler can be purged with He and hermetically sealed so the sample tray and its contents are isolated from ambient.


Kind regards,

Wolfram


-----Original Message-----
From: Stable Isotope Geochemistry [mailto:[log in to unmask]] On Behalf Of "José Manuel Moreno Rojas, PhD"
Sent: 07 October 2014 16:27
To: [log in to unmask]
Subject: [ISOGEOCHEM] Oxigen measurments in leaves and wood cellulose

Dear all,

I have been analyzing samples for groups working on tree rings (d13C) even if it is not my field of expertise (food, fraud,...). Now, those colleagues are interested on going deeper on their contact with "isotopes" and they showed their interest on analyzing d18O. Since my experience is linked to other type of samples I had several doubts:
- which are the international stds people use for that? any WS to buy somewhere?.
- which advices are given for this kind of analyses? any issues to take into account for having accurate results?.

Thank you.

Regards,

José Manuel


José Manuel Moreno Rojas, PhD
Researcher
Postharvest Technology and Food Industries Area Centro "Alameda del Obispo"
Instituto de Investigación y Formación Agraria y Pesquera (IFAPA) Avda. Menéndez Pidal, s/n. 14071 Córdoba, Spain.
tel.: +34 671532758; fax:  +34957016043
email: [log in to unmask]


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