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Dynamic Flash Combustion and High Temperature Conversion in One Elemental Analyzer
Thermo ScientificFlashEA™ 1112 HT
Elemental Analyzer for Isotope Ratio MS
m a s s s p e c t r o m e t r y
Part of Thermo Fisher Scientific
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Thermo Scientific FlashEA 1112 HT
The Thermo Scientific FlashEA 1112 HT combinestwo single-furnace systems, one for Dynamic FlashCombustion and one for High TemperatureConversion, into a single analyzer.
The Thermo Scientific FlashEA 1112 HT alsocombines the proven performance of the FlashEA 1112 and the TC/EA into one instrument.
When coupled to a Thermo Scientific Isotope RatioMass Spectrometer (IRMS), this powerful buteconomical analyzer allows bulk stable isotopeanalyses of N, C, S, H and O of organic and inorganicmaterials as well as water and other liquids.
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Today, there are more than 1000 Elemental Analyzers (EA) in use onour Isotope Ratio MS. One out of two Isotope Ratio MS sold isequipped with an EA. There is an increasing requirement for multi-element isotope analysis, including applications such as qualitycontrol and adulteration of food and drugs, environmental analysis,and forensics.
The Thermo Scientific FlashEA 1112 HT includes two complete-ly separated circuits which enable the formation and separation ofboth N2 and CO2 (in Combustion mode) or H2 and CO (in High Temperature Conversion mode). The stable isotope composition ofthese gases can be analyzed when the FlashEA 1112 HT is con-nected to a Thermo Scientific Isotope Ratio MS. Sulfur analysis isalso possible, either in simultaneous NCS analysis or in a dedicatedS mode.
The integrated TCD (thermal conductivity detector) and dedi-cated Eager 300 software allow operation of the FlashEA 1112 HTas a stand-alone instrument to determine elemental weightpercentages of N, C, H, O, and S. During isotope analysis, thedetermination of elemental weight percents is done with ourIsotope Ratio MS software, ISODAT.
The Thermo Scientific FlashEA 1112 HT comes standard with a MAS 200R carousel autosampler for solids and can optionally beequipped with either an AS3000 or GC PAL autosampler (CTC) forliquids. The FlashEA 1112 HT includes consumables for 1000analyses of each C&N and H&O. A sulfur kit is optionally available.
• Dynamic Flash Combustion- Quantitative Dumas combustion of C&N and S
• High Temperature Conversion- Quantitative reduction of O and H to CO and H2
• Multiple Isotope Analysis- 15N/14N and 13C/12C or D/H and 18O/16O, or 34S/32S
• Analysis of Solid and Liquid Samples- Organic and Inorganic Materials- Water and other Liquids
Principle of the Thermo Scientific FlashEA 1112HTThe FlashEA 1112 HT elemental analyzer facilitates multiple isotoperatio analysis by enabling conversion reactions in either of the twoseparated pneumatic circuits – Dynamic Flash Combustion or HighTemperature Conversion – with subsequent separation of the gasesin two dedicated isothermal GC columns. The ConFlo III, which isthe open split interface between the FlashEA 1112 HT and theIsotope Ratio MS, allows automated dilution of the sample gas forhighest dynamic range of C&N and H&O content and controls theintroduction of reference gases*.
Dynamic Flash Combustion and High Temperature Conversion in One Elemental Analyzer
*For more details see the Thermo Scientific ConFlo brochure
The TC/EA high temperature conversion elemental analyzer wasintroduced in 1996 and has revolutionized the measurement of 18O/16O and D/H ratios in both organic and inorganic materials.This technological breakthrough is included in the Thermo ScientificFlashEA 1112 HT. Quantitative high temperature conversion, oftenreferred to as pyrolysis or thermochemolysis, rapidly andquantitatively converts the sample’s O and H into CO and H2 in a reducing environment at high temperatures (typically exceeding1400 °C). CO and H2 are separated in an isothermal GC column prior to transfer into the ion source of the Isotope Ratio MS forsequential determination of hydrogen and oxygen isotopes of the sample.
The reactor is a glassy carbon tube filled with glassy carbongranules surrounded by a ceramic tube. The glassy carbon tubeensures that neither sample nor reaction gases make contact withthe ceramic tube to preclude oxygen isotope exchange at hightemperature. This is the only analytical technology which allowshigh precision isotope ratio monitoring of D/H and 18O/16O during a single analysis (see chromatogram below).
The TC/EA technique has been increasingly used for isotoperatio analysis of H2O. Precisions close to those of classicalanalytical techniques can be attained on sub-microliter amounts of water with analytical time of 5-6 minutes for both isotopes.
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Applications for High Temperature Conversion
• Oxygen and hydrogen analysis of organic matter
• Isotope ratio analysis of H2O
• Medical tracer studies (doubly labeled water)
• Oxygen isotopes of sulfates, phosphates, nitrates
• Nitrogen and oxygen isotopes from nitrates
• Hydrogen isotopes of phyllosilicates and amphiboles
AS3000 Autosampler for liquids
High Temperature Conversion furnace
Dynamic Flash Combustion furnace
High Temperature Conversion
Dynamic Flash CombustionThermo Fisher Scientific, Milan, Italy (formerly known as Carlo Erba)introduced the first fully automated elemental analyzer in 1968. Thislong record of continuous innovation in elemental analysis is thebasis for the Dynamic Flash Combustion mode used in the stand-alone and isotope-ready versions of the FlashEA 1112. Automatedinjection of oxygen into the reactor at a predefined time guaranteesquantitative sample conversion. The oxygen dosing is variableallowing for optimal reaction of different sample types and the mosteconomic usage of the combustion reactors.
Tin capsules used for sample introduction combust in anexothermic reaction reaching a temperature of up to 1800 °C for a few seconds. Nitrous oxides which may be formed duringcombustion are reduced by Cu to N2. After removal of H2O, the CO2 and N2 are separated on an isothermal GC column and the13C/12C and 15N/14N isotope ratios are measured sequentially. Only a few simple modifications of the combustion system are needed to change the system to SO2 for precise isotope-ratio-monitoring of 34S and 33S with high sample throughput.
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Applications for Dynamic Flash Combustion
• Authenticity control of beverages, food and drugs
• Forensic science
• Environmental Analysis
• Oceanography and limnology
• Tracer analysis
MAS 200R Autosampler for solids
Status Display
Water trap and GC cabinet withone column for N2 and CO2separation and another columnfor H2 and CO separation, TCDThermal Conductivity Detector.
FlashEA 1112 HT Elemental Analyzer for Isotope Ratio MS
Kits and Supplies
Sulfur KitBecause SO2 is adsorbed on active surfaces and can condense ontosurfaces, the analysis of sulfur isotopes requires some specializedsetups. The Thermo Scientific ConFlo III Interface is equipped with a heated Reference Gas controller which, in combination with theinert fused silica transfer lines, the heated inlet valve and theheated ion source, ensures negligible memory during analysis andallows for excellent long term performance. The Sulfur Kit includesa special reactor to optimize the combustion of bulk materials toSO2 and an SO2-inert GC column for fast sulfur analysis. The activeexhaust of the ConFlo III Interface allows excess SO2 to be ventedthrough the lab’s exhaust facility.
Tracer KitThe tracer kit allows the analysis of isotope ratios of enrichedsamples from tracer studies by extending the dynamic range of theamplifiers. The high ohmic resistors can be switched automaticallyunder computer control for analysis of isotopically enriched samplesfrom tracer experiments. The default amplification of ion beams upto 50 V covers the range from natural abundances up to 10 atom %.Above 10 atom %, a specially adapted pair of resistors is used toanalyze the highly enriched samples.
The H2O KitIsotope analysis of water and liquids by high temperature conver-sion with the Thermo Scientific FlashEA 1112 HT requires rapidtransfer of the injected liquid into the reaction zone. The H2O kitincludes a special insert for the reactor, a septum-equipped injectionhead, a microliter syringe, screw top vials and spare parts.
A special autosampler for liquids, e.g. Thermo ScientificAS3000, is recommended achieving high throughput and repeatedlyreproducible injection for highest precision.
The NoBlank optionCommon autosamplers have unsatisfactory lock systems whichallow introduction of air along with the samples, which contributesto the analytical blank. The new Thermo Scientific NoBlank Sam-pling Device for single sample purge avoids common autosamplerdrawbacks such as low sample loads, long purge times and theinability to reload carousels during acquisition. Samples are loadedinto carousels of the standard autosampler, just as before, but witheach sample drop, the NoBlank device parks a new sample from theautosampler in a small He purged chamber during analysis.
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Analytical Performance
External precision for isotope ratios C, N, S, O, H, (n=10), δ notation
Urea or acetanilide at natural abundance for C and N - IRMS13C/12C 15N/14N
50 µg C, N 0.15 ‰ 0.15 ‰0.00015 atom % 0.00005 atom %
5 µg C or 10 µg N 0.2 ‰ 0.4 ‰0.0002 atom % 0.00013 atom %
Sulfanilamide at natural abundance for S34S/32S
50 µg S 0.2 ‰
Benzoic acid natural abundance for H and O, IRMS18O/16O D/H
50 µg O, 25 µg H 0.4 ‰ 3 ‰
Water, for H and O, IRMS18O/16O D/H
0.5 µL 0.2 ‰ 2 ‰
External precision for elemental concentration (RSD)
C N H O
50 µg C, N (urea) 1 % 0.5 %50 µg O, 25 µg H (benzoic acid) 0.5 % 2 %
BR30109_E 03/07C
Thermo Electron (Bremen) GmbH is certified DIN EN ISO 2001:9000
©2007 Thermo Fisher Scientific Inc. All rights reserved.All trademarks are the property of Thermo FisherScientific Inc. and its subsidiaries.
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The Thermo Scientific FlashEA 1112 HT can beconnected to any current Thermo Scientific IsotopeRatio MS equipped for continuous flow application. If hydrogen isotope ratios are to be analyzed, the IRMSmust be equipped with an energy filter to supress 4He+ ions on the DH collector (MAT 253, DELTA V Plusand DELTA V Advantage).
Instrument description
• Base unit FlashEA 1112 HT (two furnaces)• Eager 300 software• MAS 200R Autosampler for solids with
32 sample tray• Standard outfit for H&O and N&C determination
for approx. 1000 analyses each
GasesHelium : 99.999 % purityOxygen : 99.995 % purity
Power supply230 V, 50/60 Hz, 1400 VA
Dimensions and Weight590 x 580 x 500 mm (w x d x h)67 kg (net value)
Thermo Scientific FlashEA 1112 HT Dimensions (in mm)
