1. Combustion Nitrogen Analyzers elementar Americas, Inc.
SERA-IEG Annual Meeting
June 21, 2009

2. Combustion Nitrogen Analyzers Agenda
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

3. elementar history Technology Development Organization
high temperature techniques developed in Hanau, Germany
Dennstedt Patent
Nobel prize for CHN analysis
first Macro scale elemental analyzer
first MAX analyzer
first cube platform analyzer introduced
Organization
Heraeus
management buyout forms elementar GmbH
elementar Americas Inc formed
Isoprime Ltd acquired (Isotope Ratio Mass Spectrometers)

4. 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

5. elementar Elemental 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

6. Macro N/CN Elemental Analyzers
vario MAX CN
vario MACRO CN cube
rapid N cube

7. 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

8. Elemental Analyzer Core 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 8

9. Elemental Analyzer Core 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.

10. Elemental Analyzer Core Operations
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.

11. Elemental Analyzer Chemistry
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

12. Elemental Analyzer More 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.

13. CO + CH4 ---CuO & Pt --> CO2 + H2O
Process Flow Diagram and Chemistry O2
C= 3.00%
N= 2.00%
Ash
CO2 N2 N2
NOx
CO2
sample
Ash
WO3
CO2 X- CO
H2O
CH4 O2
SO2
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.
Gripper arm removes crucible with ash from combustion tube.
Crucible deposited in recepticle for re-use
Reduction Tube
Excess oxygen reacts with Tungsten.
SO2 is adsorbed by tungsten.
Reduction Tube:
Oxides of nitrogen reduce to nitrogen gas.
Nitrogen flows to TCD.
Computer integrates peak and calculates N2 percent.
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
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
CO + CH4 ---CuO & Pt --> CO2 + H2O
Reduction
NOx + CH4+O2 +SO2--tungsten--> N2+WO3 +CO (trace)

14. 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

15. 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

16. Sample Preparation rapid 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

17. rapid N cube and vario MACRO cube
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

18. rapid N Sample Introduction Ball valve with nickle flap flange
Straight-through Ball Valve actuates.
Sample falls to top of nickel flap flange.
Nickel flap flange actuates magnetically.

19. vario MACRO cube patented 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.
More than 20 years ago we invented the ball valve technology for easy sample introduction. This patented technology is until now the best solution for this purpose. In combination with modern manufacturing and sealing materials it works without being noticed.
Picture 1: Ambient air is kept from entering the combustion tube at all times. The sample is dropped into the ball valve.
Picture 2: After one quarter turn of the ball it reaches the flush position. Ambient air inside the ball is flushed with the carrier gas (helium or argon)
Picture 3: The ball valve rotates another quarter and the sample is dropped into the combustion zone. Ambient air is still reliably blocked from the system.
Position #1
Position #2
Position #3

20. vario Max Sample preparation

21. vario MAX sample feeding

22. vario Max Sample 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

23. Analyzer Software intuitive interface easy editing
view graph during analysis
great export functionality
21CFR part11/LIMS/GLP conformity

24. 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

25. Macro sample N/CN Analyzer Selection maximum capacity (organic) and capability
1000
300
Sample
Size
200
(mg Organic
Content) 50 10 C S N CN
CNS
CHNS
CHN O Cl
Operating Mode
vario MAX
vario MAX
Rapid N
vario MAX
vario MACRO
Rapid CS
vario EL
vario TOC
vario MICRO

26. Macro sample N/CN Analyzer Selection recommendations
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

27. vario MACRO cube Elementar´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 27

28. 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) 28

29. 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
The liquid injector marks a milestone in the „cube“ family of elemental analyzers. It serves as a tool for the injection of all kinds of liquids into the cube analyzers. Within a few minutes the vario Micro cube or the vario EL cube can be turned into fully funtional CHNS analyzers for liquids.
The sample handling unit itself is mounted in the position of the solids automatic sample feeder. After exchanging the ball valve with a septum free injector port („Merlin-seal“) the sample feeder plate and attaching the gripper arm the unit is ready for operation. The entire procedure does not take longer than 10 minutes. This opens the world of liquid injections to your laboratory! 29

30. 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. 30

31. Elementar thanks you for your attention !
For further information please contact us under:
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