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Stable Isotope Lab Facility

Instrumentation

The TERRA Facility's Stable Isotope Lab operates three gas source isotope ratio mass spectrometers. Materials containing the elements of interest are converted to suitable gaseous forms and isotopic abundances are measured and compared with those of international standards.

Finnigan MAT252 Gas Source IRMS

The Finnigan MAT252 is configured for isotopic analysis of nitrogen, carbon or sulfur via continuous-flow. Interfaced with the MAT252 are a Carlo Erba NA1500 Series II elemental analyser and an OI Analytical Aurora 1030 TOC Analyser. The MAT252 also has dual inlet capabilities for isotopic analysis of prepared gas samples (N2: δ15N; CO2: δ13C, δ18O; SO2: δ34S).

ThermoElectron DeltaVPlus Gas Source IRMS

There are two ThermoElectron DeltaVPluses. DV+(I) is configured for continuous-flow isotope ratio analyses of N215N) and CO213C, δ18O). Interfaced with this DeltaVPlus are a ThermoElectron Gas Bench II, a Carlo Erba NA1500 Series II elemental analyser and an OI Analytical Aurora 1030 TOC Analyser. The DV+(II) is interfaced with an Agilent 6890N Gas Chromatograph for compound specific carbon isotope ratio analysis CO213C). It also has a dual inlet allowing for direct measurement of prepared gas samples (N2: δ15N; CO2: δ13C, δ18O; H2: δ2H).

Carlo Erba NA1500 Series II Elemental Analyser

The Carlo Erba NA1500 Series II elemental analyser is used to analyse materials for isotope ratio and elemental determinations of nitrogen, carbon and sulfur. Samples (solid inorganics and organics) are measured into tin capsules and loaded into the elemental analyser where they are then "flash combusted" with oxygen. Helium carrier gas moves the resultant gases through oxidation and reduction reactors and through a water trap. The gases then pass through a packed GC column before entering the mass spectrometer via a continuous-flow interface.

The Carlo Erba NA1500 Series II EA is interfaced through a ConfloII interface with the MAT252 for analysis of N215N, %N), CO213C, %C) or SO234S, %S). Alternately, it may be interfaced via a ConfloIII interface to the DeltaVPlus for analysis of N215N, %N) and/or CO213C, %C).

ThermoElectron Gas Bench II

The Gas Bench II is set up for analysing carbon and oxygen isotopes from carbonates. Samples are measured into glass vials and capped. The vials are placed in a heated block (50°C) and flushed with helium prior to injection with phosphoric acid. The headspace of each vial is sampled using a helium carrier gas. The resultant gases pass through Nafion® dryers and a capillary column prior to entering into the ion source.

OI Analytical Aurora 1030 TOC Analyser

The OI Analytical Aurora 1030 TOC Analyser is used for analysing water samples for inorganic and/or organic carbon content. It uses a wet chemical oxidation process to extract carbon as CO2 gas: phosphoric acid for TIC/DIC and Na-persulfate for TOC/DOC. The CO2 gas evolved from each reaction is carried by helium through a halide scrubber, water trap and Nafion® dryer before entering an NDIR detector (%C). It then passes through a reduction furnace, water trap and packed GC column allowing additional isotope ratio analysis (δ13C) in the MAT252 (via ConfloII) or DeltaVPlus (via ConfloIII).

Agilent 6890N Gas Chromatograph – ThermoElectron Combustion III Interface

The Agilent 6890N gas chromatograph is interfaced through a ThermoElectron Combustion III Interface to a DeltaVPlus allowing for the determination of carbon isotope ratios (δ13C) of individual compounds using gas chromatography - combustion - isotope ratio mass spectrometry (GC-C-IRMS). The system is currently set up for the analysis of CH4, CO2 and C1-C9 hydrocarbons in gaseous samples (manual injection) and the analysis of FAMEs (injection by autosampler). The individual compounds are separated on a GC column and directed through a combustion oven (a ceramic tube containing metal oxides at high temperature), where they are oxidized to CO2 and H2O. The water is removed via a NafionÒ dryer and the CO2 is directed into the ion source of the DeltaVplus.

Agilent 6890A Gas Chromatographs

In addition to instruments for stable isotope analysis, the lab also has two GCs for qualitative/quantitative analysis. These GCs are served by one autosampler (Gerstel MPS), which can do liquid and headspace analysis. Both GCs have a split/splitless detector.

GC A has a flame ionization detector and an electron capture detector, and is used for liquid (e.g. FAMEs) and gas (e.g. N2O) samples. This GC also has a preparative fraction collector (Gerstel PFC), which is used to isolate compounds of interest for subsequent additional analysis, such as NMR or acceleration mass spectrometry for 14C.

GC B is used for the analysis of permanent gases. This GC has a thermal conductivity detector and a flame ionization detector in series and is currently mainly used for CO2 and CH4.

Fees and Submission Requirements

Fees vary according to the type of analysis required, form and size of the sample and the preparation required. Lower rates are given to MUN grant funded and collaborative research, university and government funded analyses. Minimum sample sizes vary with procedure.

Solid samples should be dried and powdered (where possible) prior to submission. An additional fee is administered for samples that require further processing by lab personnel. For other samples, please contact the lab for requirements.

All clients should download and complete the Sample Submission form (MUN SIL Sample Submission template.xlsx) and email to Alison Pye at the address listed below.

Clients from Memorial University must also complete a Request for SI Analysis and Approval form (Request for SI Analysis and Approval.pdf) with full accounting details prior to commencing sample preparation or analysis.

Submissions from outside the Memorial University community must submit a purchase order originating from their institution or send a written request for analysis on letterhead from their institution.

 

For further information, please contact:

Ms. Alison Pye
apye@mun.ca
Stable Isotope Lab Co-ordinator
CREAIT – TERRA Facility
Memorial University of Newfoundland
Alexander Murray Building
St. John's, NL
Canada A1B 3X5
Tel: (709) 864-3217 / Fax: (709) 864-2589

For information on GC-C-IRMS analysis, contact:

Dr. Geert Van Biesen
gvanbiesen@mun.ca
ResearchLaboratory Associate
CREAIT - TERRA Facility
Memorial University of Newfoundland
Alexander Murray Building
St. John's, NLCanada A1B 3X5
Tel: (709) 864-4037 / Fax: (709) 864-2589