Frequently asked questions

By email:  [email protected]

By phone:  (613) 562-5800 ext. 6836
Lab Manager:  (613) 562-5800 ext. 6839

Shipping Address:
Ján Veizer Stable Isotope Laboratory
University of Ottawa (Science)
Advanced Research Complex
25 Templeton St.
Ottawa ON  K1N 6N5
CANADA

• Include a copy of the submission form inside the box with your samples (and the JVSIL reference number of the job if possible). Reception at times removes outer labelling and we are left with nothing to ID the samples.

• DO NOT SHIP GLASS-ON-GLASS!!! Either wrap each vial or bottle individually with bubble wrap or other padding, or make sure there is a layer of cardboard between each (if less than 50 ml) and that the content is packed tightly (no movement within the box or boxes).
• Make sure that lids will not vibrate loose; wrap lids with tape or Parafilm.
• DO NOT USE ICE CUBES for samples that need to be kept cool (not even in baggies). They melt, make a mess, and can destroy labels.  A courier may refuse to handle a leaking package, especially if there is a preservative added to the samples. 
• Insulate the entire shipment in cold weather to prevent freezing and breakage of liquid samples.
• If you are sending samples in duplicate or triplicate, it is helpful for us for them to be grouped together.
• Solid samples must be dry and powdered.
• Make sure lids are air-tight for all vials or bottles.
• Filters may be wrapped in aluminum foil, or put into wide-mouth vials (eg scintillation vials).

General rule

Since the %C is almost always larger than the %N, it is usually the %N that determines the amount of material to weigh.

In general, the equation 10 ÷ %N will give you the mg of material to weigh, targeting 100µg of N.

If that amount is larger than about 200 mg, it would be better to use 5 ÷ %N. We can even do 3 ÷ %N if needed.

If you have groups of material with quite different C:N ratios, it is best to put them in different submission files. Contact us if you need help deciding.

You must always include the %N and %C data in the submission forms, as well as the weights (if pre-weighed). We need to know the C:N in order to determine the dilution setting to use for the ¹³C analysis.

When the C:N is about 10:1 :

Please contact someone at the lab to verify the amount of material you should weigh. At this point, a compromise is needed. We reduce the normal target of 100µg of N in order to also reduce the extremely high amount of C.

When the C:N is more than about 10:1 :

At this point it is strongly recommended to run for ¹⁵N and ¹³C in separate runs. The compromise is too great to get good data in a single run.

When running for ¹⁵N, we will use a CO₂ trap to prevent the large slug of CO₂ generated in the EA from reaching the IRMS.

The rules above still apply to the weights needed for ¹⁵N.

When running for ¹³C only

A target of 300µg of C is optimal. (i.e. 30 ÷ %C). The general rule above applies to C in this case as well.  We can use less material if needed, please contact us.

Requirements

Mandatory use of 40mL pre-cleaned borosilicate amber EPA vials with septa caps (PTFE-lined silicone), purchased from a major laboratory supplier; quality assurance grade is not necessary (e.g. Fisher # 05-719-102UC; 72/cs). Please order your EPA vials early; they are often back-ordered.

NOTE: Please do not send 60 ml EPA vials. They do not fit into the carousel.

Number of replicate vials needed per sample

• Concentration (ppmC) only (no isotope analysis):
  • DIC/DOC = 1 vial per sample, filtered, full (no bubble or headspace) with extra septum
  • TIC/TOC = 1 vial per sample, full (no bubble or headspace) with extra septum
  • NOTE: pack correctly to ensure vials survive shipping as there will be no back-ups
• Inorganic C isotope analysis (DIC/TIC) only:
  • ¹³C (DIC) only = 2 identical full vials filtered (no bubble or headspace) with extra septum
  • ¹³C (TIC) only = 2 identical full vials (no bubble or headspace) with extra septum
  • NOTE: 2 replicate vials per sample is best for DCI/TIC, as a re-run on a vial with headspace can alter the 13C signal. You will also receive a concentration measurement.
• Organic C isotope analysis (DOC/TOC) only:
  • ¹³C (DOC) only = 1 vial, filtered, no extra septum. A small headspace is ok; none is best.
  • ¹³C (TOC) only = 1 vial, no extra septum. A small head space is ok; none is best.
  • NOTE: pack correctly to ensure vials survive shipping as there will be no back-ups. You will also receive a concentration measurement.
• Both Inorganic & Organic C isotope analysis (DIC & DOC or TIC & TOC):
  • ¹³C (DIC&DOC) = 2 identical full vials, filtered (no bubble or head space) with extra septum.
  • ¹³C (TIC&TOC) = 2 identical full vials, (no bubble or head space) with extra septum.
  • NOTE: Both vials need to be full and have the extra septum as we may need to use both in order to obtain the inorganic C (DIC/TIC) measurement. The organic C (DOC/TOC) can be run from the previously used vials. The two vials should be identical.
• Both Dissolved & Total, Organic and Inorganic C analysis (DIC & DOC and TIC & TOC):
  • Samples for dissolved C (filtered waters) are considered distinct from samples for total C (unfiltered waters).
  • For each sample you should provide 2 identical vials of filtered water and 2 identical vials of unfiltered water.
  • List the dissolved samples and total samples separately in each submission file. Thus if you have three separate samples (A, B and C) and you are submitting each for dissolved and total C analysis you should have six samples listed: eg. "sample A-dissolved", "sample B-dissolved", "sample C-dissolved", "sample A-total", "sample B-total", "sample C-total".
  • As above, only one media code per submission fie (organic vs. inorganic).
  • NOTE: when requesting 13C, you get a concentration measurement as a bonus (you needn't submit a separate submission file) however we still ask that you provide us with a concentration estimate (ppm-C) a priori as it guides us as to what sample volume we should use for the 13C analysis in order to fall within the mass spec's range (estimate examples: <1, <5, 5-10, 20-40, >40 ppm). And please keep in mind that when isotopes are requested the instrumentation and standards are geared to isotope analysis; the concentrations provided will thus not be as precise as in the case of a concentration only run.

Extra septum

• Samples for DIC or TIC require an extra septum (PTFE-rubber, see info below) inserted between the top of the vial and the cap. The silicone/Teflon septum provided with the EPA vials allow inorganic carbon to diffuse out unless the extra septum is used.

• We now advise that you put the darker PTFE side against the water. The rubber side of the septum can potentially affect the organic carbon. (A. Parkes (2016) verbal communication).
• The extra septum is not required for DOC or TOC; however if inorganic & organic carbon are requested, please submit 2 identical full vials with extra septum (if re-running for DIC/TIC we must use a fresh vial).

• NOTE: the septa pictured below are being discontinued.  Chromatographic Specialties has worked with a supplier to find an alternative. Contact them directly to inquire about testing the new "22mm PTFE/grey butyl septa for 24-400 Screw Cap, pk1000".

Chromatorgraphic Specialties (The original part number has been discontinued. Contact Chrom Spec for the new version that they are working on.) 
Part No. C8850522C
PTFE-rubber, 22mm flexseal disc

Labelling

• In addition to your personal label on the vial, please label each sample cap from 1 to xx in the same order as listed in the submission file. This helps us to quickly locate samples and replicates.

• Each set of identical vials should have the same number on the cap. Only enter this sample once in the submission file.
• Please include the number of replicate vials per sample directly in the submission file; either in the General Comments box if all samples have the same number of replicates or in the Comments column if the number varies.
• DO NOT use multiple layers of tape on the vial body - especially not DUCT tape - as the vials will not fit into the carousel. Please remove any excess tape before sending. The sequential number on the cap is sufficient for us if it comes to that.

Filtration

• ONLY samples for DIC or DOC should be carefully and gently filtered to 0.45 µm or less. This can be done using nitrocellulose filters (0.45 um) pre-rinsed with a minimum of 150 ml of DI water to prevent leaching of DOC from the filter. Glass fibre filters do not have the 0.45 um pore size (only 0.070 um) and also need to be pre-rinsed (M. Grinter, MSc Thesis, UOttawa, 2017). Because filtering can cause isotopic shifts due to turbulence and exposure to air, some prefer to analyse strictly TIC in order to avoid these problems.

• Samples for TIC or TOC should NOT be filtered (both dissolved and particulate C are thus analysed).
• NOTE: A filtered and an unfiltered version of the same sample water are considered two separate samples.

Flocculation

If you suspect that some of your dissolved organic matter (DOC) may have precipitated after filtration, it is possible for us to add a stir bar to the vial before analysis; however, this will incur an extra cost of $5 per sample and should be specified in the sub file.

Range of measurement

• We can analyse water samples ranging from about 0.4 to 100 ppm of carbon.
• The wet oxidation instrument (used for fresh waters and inorg. C of saline waters) allows us to select a variable volume of sample (0.5 to 8 ml) according to the expected concentration, in order fall within the mass spectrometer's sweet spot; hence the importance of providing us with all pertinent concentration info.
• Please note: organic C and inorganic C concentrations can be vastly different. Although we can obtain both C-inorg and C-org in one run, we now analyse for inorganic C first and then analyse for organic C in a second run, after sparging the samples offline.

Preservation agents

• Samples should remain refrigerated after sampling and kept cool but not frozen during shipping. Vials will be transferred to our refrigerator upon arrival.

• If the samples are refrigerated and can be shipped and analysed quickly, it is preferable to not poison the waters for preservation. We do understand that in some cases it is necessary.
• If the waters are poisoned, it MUST be clearly stated in the submission file; include the type of poison and amount.
• IF submitting only for DOC/TOC (isotopes and/or conc.) you may add acid (HCl or phosphoric) to preserve the samples, but you MUST keep the pH > 3; aim for a pH of 3-4 so as not to lose the volatile organic matter (VOM).

"Abnormal" water samples

• "Normal" samples are considered to be freshwater lake, river, groundwater, or regular seawater samples that have organic and inorganic C concentrations of less than about 80 ppm.

• If your samples are out of the ordinary in any way (i.e. very high C concentrations, high salinity, organic contamination, very high or low pH, high sulfur content, etc.), please contact us. We will let you know if we can analyse them. Our instrumentation is not adapted to handle extreme samples. Deep groundwaters tend to be problematic. If accepted, your high salinity and/or high concentration samples can be diluted with deionised water for an extra charge.
• If your sample concentrations are below our minimum ( approx. 0.4 ppm) there is nothing to be done; no isotopic data will be possible.

Submission files

• Only 1 media code per submission file: DIC/TIC (media code 42) or DOC/TOC (code 41) or ppmC-only (code 40); each requires a separate file.

• Submit a file for concentration (ppmC; media code 40) only if you are NOT submitting for isotopes.
• List each sample only once in the Sample ID column (do NOT list replicate vials unless you want them analysed too!).
• Include the number of replicate vials per sample in the Comments box at the top if the same for all, or in the Comments column if variable.
• Describe the type of waters you are submitting (e.g. lake, river, pond, ice meltwater, sea water, brines, groundwater, sediment porewater etc.).
• Include the pH & salinity data for each sample if you have it; otherwise, provide an estimate.
• Include the DIC/TIC and/or DOC/TOC concentrations (ppmC or mg/L) of each sample if you have the data; otherwise, provide an estimate (this can be from previous years in the same region or from the literature; it helps enormously in estimating sample volume to use for analysis).
• If submitting for DOC only, please include a DIC concentration estimate as well if you have it, as we may need to sparge the samples (acidification and removal of DIC) prior to analysis.
• If a preservation agent was used, include the type of agent (e.g. HgCl₂, HCl, etc) and the amount used in the general comments box.
• PLEASE REPEAT within your email message the number of samples that you are sending (including the number of replicate vials per sample) as well as the type of analysis that you wish done, for verification purposes.

Shipping

• NEVER EVER ship vials glass on glass. They WILL break.
• See sample submission (shipping) for more details.

Analysis of sediments or soils analysed for carbon is a bulk method.  The EA cannot distinguish between inorganic and organic carbon. Even a very small amount of carbonate-C can change the organic carbon ¹³C signature. See table below.

There is no perfect method. First you need to determine the type(s) of carbonate(s) present in your soil or sediment.  Calcite is easy to remove; dolomite is possible to remove with more work.  Anything more durable is extremely difficult to remove.

Do a literature search to see what method others in your field have used.  Make your choice based on this information, and on the type(s) of carbonate(s) present.

Make sure to retain some untreated material to use for N analysis if desired; any treatment of the sediment or soil can affect the nitrogen signature.  We strongly recommend running the N and C isotopes separately for best results.

Absolute Ratios (AR) of mole fractions

* Berglund, M. and Weiser, M. (2011) Isotopic Composition of the Elements 2009 (IUPAC Technical Report), Pure Appl. Chem., Vol. 83, No. 2, pp. 397–410

** Compilation of Minimum and Maximum Isotope Ratios of Selected Elements in Naturally Occurring Terrestrial Materials and Reagents, U.S. Geological Survey Water-Resources Investigations Report 01-4222 (Revised June 2002).

atm% = (100 * AR * (Delta/1000 + 1)) / (1 + (AR * (Delta/1000 + 1)))

Where AR is the Absolute Ratio (constant) and Delta is the value in permil to be converted into atm %.

Contact us for an Excel conversion calculator.

Precision Elements Ltd. offers multiple sizes of short pellet presses that are extremely useful for compressing folded capsules to remove any air, and avoid small pieces of tin/silver sticking out.  The 5mm size is perfect for 25mm GFF, and compresses almost all the air out which is difficult to do with tweezers.

Courtesy of pelletpressdiesets.com