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Combustion Nitrogen Analyzers elementar Americas, Inc. SERA-IEG Annual Meeting June 21, 2009. Combustion Nitrogen Analyzers Agenda. elementar Americas Inc. history and current organization elementar product line applications overview Analyzer technology and operation
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Combustion Nitrogen Analyzerselementar Americas, Inc. SERA-IEG Annual Meeting June 21, 2009
CombustionNitrogen AnalyzersAgenda • elementar Americas Inc. • history and current organization • elementar product line • applications overview • Analyzer technology and operation • Chemistry / Process flow / Mechanical design • Selecting an instrument • design considerations • choices - Rapid N cube / vario MACRO cube / vario MAX
elementar history • Technology Development • 1868 - high temperature techniques developed in Hanau, Germany • 1878 - Dennstedt Patent • 1925 - Nobel prize for CHN analysis • 1990 - first Macro scale elemental analyzer • 1999 - first MAX analyzer • 2006 - first cube platform analyzer introduced • Organization • 1868 - Heraeus • 1993 - management buyout forms elementar GmbH • 1999 - elementar Americas Inc formed • 2008 - Isoprime Ltd acquired (Isotope Ratio Mass Spectrometers)
elementar Organization • Manufacturing, R&D and applications labs • elementar Analysensysteme GmbH • CHNS/O Elemental Analyzers • Located in Hanau, Germany (30 minutes from Frankfurt Airport) • Isoprime Ltd • Wholly owned subsidiary • Isotope Ratio Mass Spectrometers • Located near Manchester, U.K • Sales, service, applications, and supplies • elementar Americas, Inc. • Responsible for sales and service in USA, Canada, Mexico and Central America • based in Mt. Laurel, NJ (30 minutes from Philadelphia) • Service from NJ, IN, CO, Toronto
elementarElemental Analyzer Product Line • Micro scale CHNS/O • vario MICRO cube • vario EL cube • Macro scale CHNS/O • vario MACRO cube • vario MAX • rapid N cube & rapid CS cube • TOC • liquiTOC • vario TOC cube
vario MAX CN Macro N/CN Elemental Analyzers vario MACRO CN cube rapid N cube
Elemental Analyzer Technology and Operation • Core Operations • Combustion • Gas separation • Gas detection • Chemistry • Process Flow Diagram • Other operations • Sample preparation • Autosampler and sample feeding • Software
Elemental AnalyzerCore Operations Combustion Sample combusts in furnace at 950 deg C to 1200 deg C Sample drops into crucible or is lowered into center of combustion tube Jet injection of oxygen via lance right over/at sample Creates turbulent flow around sample like blowing on a fire Three tube low voltage furnace with 10 year warranty 8
Elemental AnalyzerCore Operations • Gas Separation • Helium or CO2 carrier gas pushes combustion gases through analyzer. • C, H and S combustion gases are trapped in separate columns, then sequentially released (aka “purge and trap”). • N2 gas is not trapped. It flows straight thru columns.
Gas Detection TCD – Thermal Conductivity Detector Utilizes a Wheatstone bridge circuit to compare relative thermal conductivity differences between the carrier gas and analyte gas Critical system component Elementar own design Larger dynamic range Very special thermistors which are not harmed by high oxygen content. Allows for suspension of carrier gas flow without any harm, even at operation temperature. Elemental AnalyzerCore Operations
Elemental AnalyzerChemistry • Combustion R-N + O2 ----> N2 + NOx + O2 + CO + CO2 + CH4 + X- +SOx + H2O • Post Combustion CO + CH4 ---CuO & Pt--> CO2 + H2O • Reduction NOx+O2 +SO2--tungsten--> N2+WO3 +CO (trace) CO + CuO --------> CO2
Elemental AnalyzerMore Chemistry • Removal of other gases • X- via reaction with silver wool • H2O via condensation, membrane dryer and Sicapent • trace S02 via reaction with tungsten • Nitrogen • detected by TCD • Carbon Dioxide • rapid N – “fades” into carrier gas • vario MAX and vario MACRO – separated on purge and trap column, then released and detected by TCD.
CO + CH4---CuO & Pt --> CO2 + H2O Process Flow Diagram and Chemistry O2 C= 3.00% N= 2.00% Ash CO2 N2 NOx N2 CO2 Ash sample WO3 CO2 CH4 O2 H2O SO2 CO X- CO2 Oxidation ----> CO + CO2 + CH4 + N2 + NOx + SOx+ H2O + X- + O2 X X X X X X X • R-N + O2 Post Oxidation • CO2 column is heated. • CO2 flows to TCD. • Computer integrates peak and calculates CO2 percent. • Reduction Tube: • Oxides of nitrogen reduce to nitrogen gas. • Nitrogen flows to TCD. • Computer integrates peak and calculates N2 percent. • Reduction Tube • Excess oxygen reacts with Tungsten. • SO2 is adsorbed by tungsten. • Combustion gasses are produced • We are interested in N2 and CO2. • Other gases must be converted or removed. • Halogens are removed by reaction with silver wool in post combustion tube. • Gripper Arm lowers crucible containing sample into combustion tube • Oxygen is injected over sample • Sample combusts • Gripper arm removes crucible with ash from combustion tube. • Crucible deposited in recepticle for re-use • Methane and carbon dioxide are oxidized in post combustion tube. • Carbon dioxide flows through instrument and is trapped in column • Water is removed by a three stage dryer: • condensation • membrane dryer • Sicapent Reduction • NOx + CH4+O2 +SO2--tungsten--> N2+WO3 +CO (trace)
Process Flow Diagram Comparison Replace robotic arm with Carousel and ball valve Add CF Hybrid vario MACRO cube CN Replace robotic arm with Carousel and ball valve CO2 Remove CO2 adsorber Rapid N cube
Elemental Analyzer Technology and Operation • Core Operations • Combustion • Gas separation • Gas detection • Chemistry • Process Flow Diagram • Other operations • Sample preparation • Autosampler and sample feeding • Software
Sample Preparationrapid N cube and vario MACRO cube 60 position open carousel - add samples at any time during run - optional 80 or 120 position carousel Variety of foils/capsules Sample Pressing Tool
Ball Valve Sample Feed rapid N cube and vario MACRO cube • rapid N cube and vario MACRO cube have slightly different designs. • Both designs provide: • inherent blank-free system • reliable function • keeps air out of the system • very long lasting operation • easy maintenance
rapid N Sample IntroductionBall valve with nickle flap flange • Straight-through Ball Valve actuates. • Sample falls to top of nickel flap flange. • Nickel flap flange actuates magnetically.
vario MACRO cubepatented zero-blank ball valve • Position 1; Sample falls into ball valve cavity. • Position 2; Ball valve cavity purged with helium. • Position 3; Ball valve opens to combustion tube. Position #1 Position #2 Position #3
vario MaxSample Feeding • Robotic “gripper arm” • Lifts reusable crucible from carousel. • Lowers crucible into the combustion tube (~1000o C) • Lifts to removes crucible and ash • Deposits the ash & crucible in catch bin
Analyzer Software • intuitive interface • easy editing • view graph during analysis • great export functionality • 21CFR part11/LIMS/GLP conformity
Elemental Analyzer Technology and Operation • Core Operations • Combustion • Gas separation • Gas detection • Chemistry • Process Flow Diagram • Other operations • Sample preparation • Autosampler and sample feeding • Software
Macro sample N/CN Analyzer Selection maximum capacity (organic) and capability vario MAX vario MAX Rapid N vario MAX vario MACRO Rapid CS vario EL vario TOC vario MICRO
Macro sample N/CN Analyzer Selectionrecommendations • Vario MAX • Best choice for CN or N samples that are non-homogeneous, very low in concentration, wet , high ash or difficult to handle. • Vario MACRO cube • Optimum economics for larger CN samples with easier handling characteristics (dry, semi-homogeneous). • Capital cost lower than MAX • CF Hybrid technology optimizes consumables cost • Rapid N cube • Optimum economics for larger N samples with easier handling characteristics. • Capital cost lower than MACRO • CO2 carrier gas reduces gas cost
vario MACRO cubeElementar´s answer to YOUR analytical needs • The new cost-effective macro analyzer family for • N/CN for protein, plant material or soil analysis • CNS • CHNS for plant and soil, environmental or oil samples • CHN for the analysis of coal, biomass or combustible solid waste
Options: • „Standard options:“ • Capsule press for liquids • Pressing tool • IR Detectors for special applications: • low level sulfur analysis • low level oxygen analysis • chlorine analysis • VLS, vario liquid sampler • Continuous flow Hybrid (CN only)
Options:Automatic liquid injector for the „cube“ family • liquid sample feeder for 60 samples, plus flushing and waste positions • easy setup, replaces standard ball valve and carousel • can be used on: • vario EL cube • vario MICRO cube • vario MACRO cube • Launched in 2008, first installations successful
CF-Hybrid technique for CN mode • The newly developed hybrid technology serves for longer lifetime of consumables. • Only a fraction (approx 50%, adjustable) of the combustion gas is lead through the reduction tube in continuous flow mode, saving valuable reduction metal and expansion of uninterrupted operation time. • Features: • Easy to install and remove (1-2 minutes!), so the user can choose between highest sensitivity or highest throughput. • Active flow control. • Ideal for high-throughput laboratories with similar sample matrix.
Elementar thanks you for your attention ! For further information please contact us under: Web Page: www.CHNOS.com e-mail: info@elementar-inc.com