Finnigan Delta Plus XP

The Finnigan DELTAplusXP is the universal routine and research stable isotope ratio mass spectrometer for all applications using dual-inlet and continuous-flow techniques. Its extended image plane supports continuous flow D/H measurements as well as the determination of atmospheric gases. The amplifier dynamic range is 50 V.

• The DELTAplusXP is a universal tool for ¹³C/¹²C, ¹⁵N/¹⁴N, ¹⁸O/¹⁶O, ³⁴S/³²S, ³⁷Cl/³⁵Cl, and D/H determination in dual inlet and continuous flow modes.
• The DELTAplusXP offers simultaneous acquisition and ratio evaluation on up to eight Faraday collectors on a single image plane with a mass range of 22 %, e.g. m/z 28 - 44 or m/z 2 and 3. It has the widest flexibility in detector configurations allowing development of novel applications but with no compromise to the traditional applications.
• The DELTAplusXP is optimized for the on-line measurement of D/H isotope ratios in a He carrier gas stream, with the complete suppression of 4He+-interferences on m/z 3 (HD).
• The DELTAplusXP provides a flexible and open platform for the connection of inlet systems and preparation devices. Full integration of the ISODAT 2.0 gas isotope data system enables easy set up, tuning and automatic operation of the DELTAplusXP.
• The powerful ISODAT 2.0 ISL Script Language provides access to all processes, and allows modification of supplied scripts as well as development of entirely new measurement and evaluation protocols.

Finnigan GasBench II

The GasBench II is a continous flow preparation device and inlet system with repetitive loop injection of gases. Supported by a GC-PAL autosampler and using septum-sealed sample vials, a wide variety of applications are accessible for high precision on-line measurements. The GasBench II connected to a DELTA PLUS XP offers precision comparable to dual inlet methods for H₂ and CO₂ water equilibration, CO₂ from air, and dissolved inorganic carbon but with the enhanced productivity and ease-of-operation of Continuous Flow Isotope Ratio Mass Spectrometer. Although the GasBench II is capable of several measurement types, we are currently using it for the following analyses: ¹⁸O/¹⁶O via water equilibration, ¹⁸O/¹⁶O and ¹³C/¹²C from carbonates, ¹³C/¹²C from dissolved inorganic carbon in water, and ²H/¹H via water equilibration.

Elemental Analyzer

The ConFlo III Interface allows the connection of a wide variety of elemental analyzers to the DELTA PLUS XP including quantitative high temperature carbon reduction (pyrolysis) elemental analyzers for analysis of D/H and ¹⁸O/¹⁶O (TC/EA) and a Carlo Erba NA1500 elemental analyzer (EA) deigned for the measuremnt of ¹⁵N/¹⁴N and ¹³C/¹²C. The TC/EA can make measurements for liquid or solid sample matrices using either a CTC GC-PAL autosampler for automated injection of water samples or a Costech zero-blank autosampler for introduction of solid samples (i.e. cellulose, feather, hair). The NA1500 EA is equipped with an AS200 pneumatic autosampler with a minimal blank interference. Both devices are plumbed to the DELTA PLUS XP for high percision measurements. Both peripheral devices are capable of making both quantitative and isotopic measurements.

Finnigan MAT 252 IRMS

With the Finnigan MAT 252 you can perform gas isotope ratio measurements of H/D, ¹³C/¹²C, ¹⁵N/¹⁴N, ¹⁸O/¹⁶O, ³²S/³³S/³⁴S.

The basic instrument is equipped with a dual inlet system for classical applications. It is of a modular design for the adaptation of different inlet modules thus enabling a configuration of the instrument tailored to the requirement of the users. The sample side can be connected to:

• A second inlet system for variable sample volumes, a multiport with or without a tube cracker installation,
• Microvolumes for very small samples,
• Multisample inlets for separating and purifying samples or,
• Installations for "on-line" coupling to gas chromatographs, elemental analyzer or other peripherals.

Inlet System for MAT 252

The configuration of the inlet system of the MAT 252 mass spectrometer is of asymmetrically design to enable alternately measurements of a sample and a standard gas.

The instrument is equipped with a dual inlet system with a configuration identical for the sample and standard side which enables a balanced intake. Each inlet side has two ports and a variable volume with the respective inlet capillary leading to the changeover valve. For very small samples a microvolume with its own capillary is installed.

Peripherals for MAT 252

ConFlo III Interface

The ConFlo III Interface provides the means for coupling the EA to the IRMS. The connection of the Elemental Analyzer with an isotope ratio mass spectrometer via an open split arrangement has become standard for on-line isotope ratio analysis. The IRMS works with helium flow of ~0.03 ml/min, this gas flow is the central idea of the open split arrangement.

The Open Split Principle

The size of the IRMS capillary determines a 0.3 ml/min gas flow to the mass spectrometer. This MS capillary continuously "sniffs" the carrier gas (He) flowing through the cell. The carrier gas flushes the open split cell continuously with helium and passes the gaseous sample so transporting the produced compounds consecutively through the cell.

Procedure for the ConFlo III Interface

The ConFlo III Interface forms an innovation in coupling an Elemental Analyzer to an IRMS in the way that two separate open split cells replace the "tube in tube" samples gas inlet performed in the predecessor model ConFlo II.

Through the separation of the sample stream and the reference inlet, ConFlo III forms a dynamic and flexible way of an EA/IRMS connection. These two open split cells allow a higher precision of on-line determination as well as a temporal independent sample/reference gas introduction to the IRMS.

CosTech ECS 4010 Elemental Analyzer

The ECS 4010 Nitrogen / Protein Analyzer was designed as an advanced analytical platform for CHNSO elemental analysis and Nitrogen / Protein determination. It is based on an automatic analytical unit whose operation - from sampling up to signal detection - is microprocessor controlled. It represents an evolution in the technique of elemental analysis by "flash combustion/chromatographic separation and multi-detector techniques".

Traditionally, automatic instruments for CHNSO elemental analysis have been divided into two groups; micro and macro elemental analysis. Samples for micro EA are easily analyzed by sophisticated automatic instruments using the technique of combustion/gas chromatography.

For the analysis of stable isotopes of CHNSO, a sampling system is required which does not contaminate the sample with atmospheric nitrogen and oxygen, especially working at very low levels. Advanced, highly stable catalysts are required to avoid any material exchange to the combusted gases.

To increase throughput and minimize maintenance time and cost, a simple approach to the design of the analyzer is essential, especially for macro sample analysis where all combustion gases pass through the detector system without splitting or diluting.

ECS 4010 Description:

Starting from the basic furnace design; the ECS 4010 has two, large capacity (up to a 26 mm OD reactor) furnaces. Optional fittings let you quickly and easily switch between combustion/reduction reactors of different diameters. You can work with reactors from 10,5 mm to 26 mm OD.

The furnaces are mounted in a specially designed SS enclosure with an extremely efficient insulating material. This keeps the entire cabinet "cool to the touch" and allows the furnaces to heat from ambient to operating temperature in 1.5 hours. The electronics and power supplies are completely isolated from the furnace compartment and have their own separate cooling fan. The ECS monitors, and can display, the temperatures of the power supply, and electronics. It will also display the input line voltage supply.

The ECS 4010 consists of three modules:

The first module is the combustion system, the second is the detector system, and the third is the data handling system. When the three systems are combined the user can choose the required analytical configuration.

The first module consists of sampling, combustion and pneumatics. The autosamplers available are a sealed, "Zero Blank" sampler, and an open carousel sampler, where samples can be added continuously. The movement of the "Zero Blank" autosampler is controlled by a microstepping motor. You can choose either a 32 or 50 position carousel through the instrument software, and since it is completely sealed to atmosphere there is no contamination of the samples from nitrogen or oxygen. This is especially useful for stable isotope analysis. The second choice of sampler has carousels which are open to the atmosphere, but samples can be added continuously and the number of sample positions is 147.

The ECS 4010 is equipped with two furnaces. Temperature control of the combustion furnace is up to 1100 °C, and the reduction furnace 800 °C. The furnace dimensions and special fittings allows you to use a wide variety of reactors to tailor the analyzer to your laboratory needs (small and large samples, CHNSO analysis, and N/Protein). The connection fittings for the quartz reactors make it fast and easy to replace the inserts in the combustion reactors (removal of ash and residue), for longer tube and catalyst life. The unique pneumatic system can be switched between three operating modes; Micro, Semi-Micro and Macro. By selecting a mode you choose the volume of oxygen for sample combustion. The gases (helium, oxygen and servo) are controlled by reliable SS diaphragm regulators for accurate flow control. Servo gas control is provided for use with our pneumatically actuated autosampler. A separate purge regulator is provided for flexibility in purge gas flow and volume.

The second module is the detector system for measuring the combustion (or pyrolysis) products. These combustion gases can be separated by gas chromatography for CHNSO analysis, or sent to a mass spectrometer for isotopic analysis. For the gas chromatographic technique a high stability oven, with temperature control from 30-110 °C, and a wide range of GC column lengths are available. The TCD (thermal conductivity detector) has been specially designed for this application, special features include; preheating of combustion gases before entering the detector to stabilize gas temperature, and a twin encapsulated filament which requires no reference gas flow.The advantages of the this are; simplicity of the combustion/detector system (low maintenance, minimum down time), efficiency of the combustion, and no splitting or dilution of the combustion gases, all combustion products are measured.

The third module is EAS32, our WindowsTM based software package, for instrument control, data acquisition and report generation. A multichannel 32 bit A/D interface connects the ECS to a PC for data acquisition. Sample information is entered, the software collects raw data from the TCD, creates the calibration, and generates reports. Data can be easily exported to EXCELTM in ASCII format for postrun calculations or exporting to LIMS. A reprocessing software option is available for setting up methods and transferring data from a remote computer, or working with data out of the laboratory. Interface boards can be ordered for 1, 2 or 4 channels. 

Thermo Scientific MAT 253 Isotope Ratio Mass Spectrometer (IRMS)/ Kiel IV

The Thermo Scientific MAT 253 stable isotope ratio mass spectrometer system delivers the highest precision for the determination of H/D, ¹³C/¹²C, ¹⁵N/¹⁴N, ¹⁸O/¹⁶O, ³⁴S/³²S (from SO₂ and SF₆), ²⁸Si/²⁹Si as well as Ar, Kr, and Xe isotope ratios.

Information for MAT 253 IRMS

• Computer switchable amplifier gain
• Hydrogen continous flow capability
• Highest sensitivity and linearity
• "Fast Bellows" system
• Computer-controlled ion source potentials and parameters
• Up to eight simultaneous acquisition channels
• "Plug and measure" peripheral recognition
• Small footprint and proven robustness
• Easy set up, tuning and fully automatic operation
• Ion source with variable conductivity
• All-metal sealed ion source and analyzer
• Monolithic all-metal valves with gold gaskets
• 100% anaylzer transmission
• Mass resolution 200 (C,N,O,S)
• Only system for e.g. SF₆, SiF₄, Xe
• Isodat Script Language (ISL) provides access to all processes and allows modification of supplied scripts as well as development of entirely new measurement and evaluation protocols

Specifications for MAT 253 IRMS

• Mass Range 1 to 150 dalton at 10kV
• Resolution CNOS: m/delta m = 200 (10% valley), HD: m/delta m = 25 (10% valley)
• Peak Top Flatness better than 2 X 10e^-4
• Sensitivity (absolute) 600 molecules CO₂ per mass 44 ion at the collector (600 molecules.ion)
• Abudance Sensitivty: the contribution of the mass 44 intensity to the intersity of mass 45 is less than 2 x 10e^-6
• Sample Consumtion 0.031nmol/s for 1.5V signal (5nA) at mass 44 in the Dual Inlet mode 0.047nmol/s for 1.5V signal (5nA) atr mass 44 in the Continous Flow Mode
• Ion Source Linearity 0.02%/nA ion currnet (mass 44) at a sensitivity corresponding to 900 molecules/ion
• H3+ Factor smaller than 10ppm/nA

KIEL IV

Information for Kiel IV

Isotope ratio analysis of carbonate samples is increasingly important in paleoclimatic reconstructions. The requirement for isotope ratio anaylsis of small samples of carbonate arose in studies of biogenic carbonates (e.d. foraminifera, bivalves, brachiopods, otoliths, corals). Studies of carbonates from growth zones of individual organisms and high resolutionm studies of microfossils from drill cores require an analytical system which can provide both high throughput and high performance in precision and accuracy over a large dynamic range of sample size.

The KIEL IV Carbonate Device coupled to the 10-kV Thermo Scientific MAT 253 isotope ratio mass spectrometer meets the requirements of such work by providing the highest linearity at highest sensitivity, while enabling high throughput through full automation of the analytical process, from the resaction to the reporting of measurement results.

The KIEL IV Carbonate Device uses the principle of individual acid baths. Storage, transfer, and chemical reaction of phosphoric acid at elevated temperatures operate under full temperature control. CO₂ evolves in septum-free vials and diffuses under medium vacuum pressure into a crypgenic trapping system. Water and noncondensable gases evolved during phosphorolysis are removed from the CO₂ gas phase under high vacuum in the first trap. Prior to transfer into the microvolume, the CO₂ pressure is monitered and, if required, the CO₂ sample size can be reduced by expansion into a defined volume. In the microvolume, the dry CO₂ is prepared for analysis in a dual microvolume inlet system which features a new design of the microvolume on the sample side.

Analytical Performance

With a sample size of > 25μg for MAT 253 the following performance for one full autosampler run (46 samples) will be achieved

External Precision 1 σ

Carbon (¹³C/¹²C) 0.03‰

Oxygen (¹⁸O/¹⁶O) 0.07‰