FP628. Nitrogen / Protein Determination by Combustion. Rev 1-6/8/11

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1 FP628 Nitrogen / Protein Determination by Combustion Rev 1-6/8/11

2 Presentation Outline LECO Background N Determination FP628 Theory of Operation Specifications Advantages Software Data

3 LECO Background Privately owned U.S. Company for over 70 years Headquartered in Saint Joseph, MI Diverse Instrumentation offerings Organic and Inorganic Elemental Analysis Mass Spectrometry (TOF) Metallography Microscopy and Image analysis Environmental Food Energy Metals Mining 25 LECO subsidiaries representing over 100 countries

Instrumentation offerings Organic and Inorganic Elemental Analysis Mass

4 N / Protein Determination Quantitative Analysis Nutritional labeling (protein) for foods and feeds Material characterization - education/research, commercial and regulatory Soil/plant science Process and Quality Control Grade and value for feeds Food, agricultural and chemical processing Milling applications (starch, flour, oilseeds) Chemical and Specialty materials processing (resins, adhesives, etc)

and Quality Control Grade and value for feeds Food, agricultural and chemical processing Milling

5 Techniques for Determining Nitrogen

6 FP628 Vertical quartz furnace tube with a maximum temperature of 1050 C Sample mass 50mg up to ~1g Tin capsules or foils used to encapsulate sample and attain high combustion temperature ~1800 C Reticulated crucible collects ash from sample and tin cap or foil

encapsulate sample and attain high combustion temperature ~1800

7 FP628 Theory of Operation A sample is weighed into a foil or capsule and loaded into autoloader

8 FP628 Theory of Operation Sample is loaded into purge chamber removing atmospheric gas Sample introduced to furnace

9 FP628 Series Theory of Operation Combustion gases are swept from the furnace into the thermo electric cooler Moisture efficiently removed without the use of chemical anhydrone

10 FP628 Theory of Operation Combustion gas is swept onto the combustion gas collection and aliquot collection system

11 FP628 Theory of Operation Aliquot gas is swept through a reduction reagent tube then passes through Lecosorb and anhydrone reagent tube

12 FP628 Theory of Operation The aliquot gas passes through a thermal conductivity cell for nitrogen detection

13 Thermal conductivity table

14 FP628 Specifications Instrument Range Nitrogen 80ppm to 100% 500mg Precision Range Nitrogen 0.02 mg Nitrogen or 0.5% RSD (whichever is greater) Analysis Time ~4.5 minutes nominal Sample Mass N up to ~1g, 500 mg nominal Cost per Analysis ~54p regardless of sample weight, type, moisture

5% RSD (whichever is greater) Analysis Time ~4.

15 FP628 Series Specifications (cont.) Detection Technique Nitrogen Thermal Conductivity (TC Cell) Detector Furnace Resistance Primary and Secondary up to 1050 o C max Autoloader 30-position, expandable up to 120 Electrical Power Requirements Instrument 230 V~, 50/60 Hz, single phase, 12A

Furnace Resistance Primary and Secondary up to 1050 o C max Autoloader

16 Instrument Range Concentration Calc FP628 range: 500 mg sample mass Nitrogen (80ppm to 10%) Low end = (0.04 mg N / 500 mg sample) * 100 = 0.08% or 80 ppm N High end = (50 mg N / 500 mg sample) *100 = 10% N

17 FP628 Advantages Analysis Time Throughput Analysis time FP628 is the fastest macro combustion instruments in the market FP628 Series analysis time is ~4.5 minutes Whole gas analysis techniques using chromatographic separation or purge and trap approached typically have 2 times longer analysis times Competitive whole gas instruments analysis times are dependent on element configuration and sample mass (more elements and or sample mass = longer time ) Samples/Hour FP628 Series 14 Competitor N model 7

5 minutes Whole gas analysis techniques using chromatographic separation or purge and trap approached typically have 2 times

18 FP628 Advantages Low cost-per-analysis Exclusive use of Oxygen within Combustion Furnace results in: Ensures complete combustion and superior recovery of elements Speeds combustion Allows for use of macro sample mass Eliminates the need for other reagent oxidizers within combustion system Ballast and Aliquot Combustion Gas Handling system Allows for the exclusive use of pure oxygen in the furnace Eliminates treating the whole combustion gas with CO2 scrubbers and reduction reagents Significantly extends lifetime of CO2 scrubber and reduction reagents

combustion system Ballast and Aliquot Combustion Gas Handling system Allows for the exclusive use of pure oxygen in the furnace Eliminates

19 FP628 Advantages Ability to determine carbon hydrogen and nitrogen in macro samples of various organic matrices under the same method and conditions Multiple methods and calibrations are not required to compensate for poor combustion conditions Allows system to analyze heterogeneous samples with better precision and accuracy Plant Tissues Feeds Flour Etc.

calibrations are not required to compensate for poor combustion conditions Allows system

20 FP628 Series Software LECO Windows -based operating software Seamless management of data and detector plots Integrated control charts and statistical calculations

21 FP628 Series Software LECO Windows-based operating software Monitor real-time internal component readings Expanded interactive diagnostic screens aiding Troubleshooting Improve serviceability

22 FP628 Series Software LECO Windows-based operating software Simplified data handling with convenient storage and customizable reporting and data exporting capabilities User definable fields for automatic calculations Compatible with various Laboratory Information Management Systems (LIMS)

23 FP628 Calibration Wide Dynamic Range Calibration ~50 mg to ~350 mg EDTA 1.0 to 33.5 mg N Linear curve type

24 CN628 Blanks Low Consistent Blank ~3 ppm Nitrogen Std Dev

25 FP628 Data Corn Flour Sample Data ~250 mg sample mass EDTA Calibration Cert values: / % N

26 FP628 Data Corn Flour Sample Data ~250 mg sample mass EDTA Calibration Cert values: / % N

27 FP628 Data Glycine Solution Sample Data ~300 mg sample mass EDTA Calibration Expected value: 0.1 % N

28 FP628 Data Ammonium Sulfate Sample Data ~50 mg sample mass EDTA Calibration Theoretical value: 21.2 % N

29 CHN628 Series Elemental Analysis by Combustion Unparalleled Capabilities

30 Leco Macro Nitrogen Determination Vertical and horizontal furnace designs utilize the LECO combustion approach resulting in: Rapid analysis time (4 minutes) Extended reagent lifetimes and instrument uptime Ability to handle macro samples up to ~3g Low cost-per-analysis Complies with AOAC, ASTM, ISO, AACC AND ASBC approved methods

31 Leco Instruments UK Ltd Thanks for Listening Michael Reaney If you require further information please feel free to contact the Leco stand

DETERMINATION OF TOTAL CARBON, TOTAL ORGANIC CARBON AND INORGANIC CARBON IN SEDIMENTS

DETERMINATION OF TOTAL CARBON, TOTAL ORGANIC CARBON AND INORGANIC CARBON IN SEDIMENTS Bernie B. Bernard, Heather Bernard, and James M. Brooks TDI-Brooks International/B&B Laboratories Inc. College Station,