Nu Perspective IRMS

The Nu Instruments Nu PERSPECTIVE IRMS is a state of the art stable isotope ratio mass spectrometer designed for flexibility, high performance, and reliability, together with a user friendly instrument control software and data analysis suite.

 

This next generation instrument has a wealth of novel features, giving the ultimate in performance for both routine and research applications for stable isotope ratio measurements.

 

The combination of the analyser geometry- field proven in the Nu Instruments Noblesse noble gas mass spectrometer- and the use of the “zoom optics” (Nu patent) gives an equivalent dispersion for CO2 of 60cm – the largest in any commercially available IRMS instrument.

 

The ion source sensitivity in dual inlet mode has been determined at <600 molecules/ion (for CO2 at mass 44) at 10kVz

 

 

Nu PERSPECTIVE ion source

 

  • All ion source parameters are under computer control, with storage of the tuning parameters for each sample gas and isotope ratio to be measured.

  • The ion source has integral focussing lenses (bidirectional focussing in both the vertical and horizontal planes) giving 100% transmission of ions through the analyser.

  • Low (<10ppm/nA) and stable (<0.03 ppm/nA/hour) H3+ formation- essential for precise D/H analysis

  • Integral ion source heater (temperature up to 200oC)

 

Nu PERSPECTIVE magnetic sector analyser

  • Variable mass dispersion of up to 60cm effective magnetic deflection radius (varies with the use of the patented zoom lens)

  • Mass range 2 to 150, mass resolution (m/Δm, 10% valley) >200

  • Simultaneous collection of from 2 to 6 ion beams, with 10 collectors fitted as standard to permit the simultaneous measurement of either masses 2,3; 28,29,30; 44,45,46,47,48,49; or 64,65,66,68

  • High stability electromagnet supplied as standard

  • High efficiency, narrow entrance, and deep Faraday collectors are used, that uniquely provide high resolution on all collectors

  • The combination of the analyser geometry and electromagnet gives high spatial separation of masses 2 and 3, allowing the measurement of D/H ratios in H2 in a helium carrier gas without the need for any additional ion optic elements

Nu PERSPECTIVE vacuum system

  • True differential pumping is supplied as standard, by three BOC Edwards EXT75 70 litre/second water cooled long lifetime turbomolecular pumps, with high compression ratio for pumping of light gases (e.g. He and H2). One BOC Edwards rotary backing pump, floor standing (inside the PERSPECTIVE cabinet)

  • Penning gauge for measurement of ion source pressure, with computer monitoring of both turbomolecular pump rotation speeds and temperatures, with automatic shutdown in the case of vacuum failure

Nu PERSPECTIVE instrument control and data acquisition electronics

 

  • Single module ion source supplies unit, fully computer controlled

  • Rack mounted data acquisition and control PCBs mounted in separate and isolated module

Nu PERSPECTIVE data system and software

  • Comprehensive and easy to use Windows® based control software

  • Full colour display of all operating parameters, e.g. ion beams, pressure gauge

  • True multitasking operation

Nu PERSPECTIVE reference gas injection and continuous-flow IRMS interfacing

  • Reference gas injection system for 5 gases (CO2 N2,H2, CO, and SO2)

  • Computer controlled dilutor (variable from no dilution up to 30x dilution)

  • Pneumatic isolation valve to isolate the ion source

Installation Requirements

  • Dimensions cm (width) x cm (depth) x cm (height)

  • Single phase power supply 230V/15A required

  • Compressed air @ 90psi for pneumatic valves

  • Closed loop water chiller/recirculator (for turbomolecular pump cooling).

Nu PERSPECTIVE Continuous Flow IRMS performance specifications

 

EA-IRMS mode -sample combustion to CO2, N2, or SO2 with EuroVector Elemental Analyser

 

Gas and isotope ratio

 

Reference Gas Precision

(1σ, n=10, 15nA peaks)

EA-IRMS external precision (1σ, n=10)

Sample Size (absolute elemental amount in capsule)

CO2 (13C//12C)

0.06‰

0.1‰

50µg

CO2 (13C/12C)

 

0.3‰

15-300

N2 (15N/14N)

0.06‰

0.1‰

50µg

N2 (15N/14N)

 

0.3‰

20-400µg

SO2 (34S/32S)

0.1‰

0.1‰

50µg

 

Pyrolysis mode –solid or liquid sample pyrolysis to CO and H2 with a HEKAtech Unit 1700oC High Temperature Carbon Reduction Furnace

 

Gas and isotope ratio

Reference Gas Precision

(1σ, n=10, 15nA peaks)

Pyrolysis external precision (1σ, n=10)

Sample Size (absolute elemental amount)

H2 (D/H)

0.2‰

3‰

25µg (solid)

H2 (D/H)

 

3‰

30-150µg (solid)

H2 (D/H)

 

2.0‰

0.5µl (liquid)

CO (18O/16O)

0.1‰

0.3‰

50µg (solid)

CO (18O/16O)

 

0.6‰

25-250µg (solid)

CO (18O/16O)

 

0.2‰

0.5µl (liquid)

 

Nu Instruments GC-combustion/pyrolysis-IRMS interface

For on-line measurement of δ 13C, δ 15N and δD in organic compounds that are separated by capillary gas chromatography. The helium carrier gas is switched between the FID or the combustion / pyrolysis of components of interest in an oxidation or pyrolysis furnace.

 

Water is removed from the products of combustion using a Nafion dryer.

 

For δ15N measurements any N oxides are reduced to N2 using a low dead volume reduction furnace and CO2 is removed using a low dead volume liquid N2 trap.

 

Pulses of pure reference gas are automatically introduced into the HORIZON ion source for best possible precision and accuracy.

 

N.B. when determining δD via the high temperature pyrolysis furnace, at the start of the GC run 3 (or more) reference gas peaks of H2 are introduced at different major ion beam values to determine automatically the H3+ correction for the GC run.

 

The GC combustion/pyrolysis interface includes:

 

An Agilent Technologies 7890A Gas Chromatograph fitted with one capillary split/splitless injector and EPC

 

One Flame Ionisation Detector (FID) fitted with heart cut valve

 

Oxidation furnace, interfaced to the 7890A, with temperature controller (maximum temperature 1200oC)

 

Pyrolysis furnace, interfaced to the 7890A, with temperature controller (maximum temperature 1450oC)

 

The combination of the Agilent 7890A GC together with the PERSPECTIVE IRMS meets the following specifications:

 

Precision <0.2‰ for δ13C, <1.0‰ for δ15N, and <3‰ for δD

 

For the measurement of δ13C the above precision is met with >0.8 nanomoles (10ng) of C on column; for δ15N >1.5 nanomoles (42ng) of N2 on column; and for δD >15 nanomoles (30ng) on column.

Included will be a 30m DB-5MS 0.25mm x 0.25µm GC column

 

Optional autosamplers available include the Agilent 7693A, CTC GC PAL & COMBI PAL units, and the Gerstel MPS2L

 

ADDITIONAL SAMPLE PREPARATION ACCESSORIES

 

Nu Instruments “GasPrep” System

 

Continuous Flow Water Equilibration & Carbonate/Phosphoric Acid Reaction System

 

A Nu HORIZON system installed in the KISR, Kuwait (GasPrep System in the centre)

 

Nu Instruments has developed a new sample preparation unit to be used with the Nu PERSPECTIVE and Nu HORIZON Isotope Ratio Mass Spectrometer instruments.

 

The unit uses an autosampler similar to the Gilson Model 222XL, and is fitted with a temperature controlled block that can house up to 100 industry standard “Exetainer” septum capped glass vials.

 

When used for equilibration of water (H2O) with either CO2 (for 18O/16O analysis) or H2 (for D/H analysis) the performance specifications, (when used with a PERSPECTIVE or HORIZON IRMS in continuous flow mode of operation) are as follows:

 

δ18O (as CO2) Sample Size >500µl H2O External Reproducibility <0.1‰

 

δD (as H2) Sample Size >200µl H2O External Reproducibility <2.0‰

 

The unit can also be used to sample CO2 prepared from carbonate samples (e.g. DIC, solid carbonates) by the addition of phosphoric acid to the carbonate samples followed by automated determination of 13C/12C and 18O/16O ratios.
 

In carbonate mode the specifications are:

 

δ18O (as CO2) Sample Size >50µg CO32- External Reproducibility <0.08‰

 

δ13C (as CO2) Sample Size >50µg CO32- External Reproducibility <0.06‰

Kontakt

HEKAtech GmbH

Friedrich-List-Allee 26

41844 Wegberg

Germany

 

Tel.: +49 (0)2432 49 36 49

Info@HEKAtech.com