APA Conference 2011 Presentation Leco

8/12/2019 APA Conference 2011 Presentation Leco

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FP628

Nitrogen / Protein

Determination by Combustion

Rev 1 - 6/8/11



Presentation Outline

• LECO Background

• N Determination

• FP628

– Theory of Operation

– Specifications

– Advantages

– Software – Data



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

• 25 LECO subsidiaries representing over 100 countries

Food

Energy

Mining

Environmental Metals



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)



Techniques for Determining Nitrogen



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



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



FP628 Theory of Operation• Sample is loaded into purge chamber

removing atmospheric gas

• Sample introduced to furnace



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



FP628 Theory of Operation• Combustion gas is swept onto the

combustion gas collection and aliquot

collection system



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

and anhydrone reagent tube



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



Thermal conductivity table



FP628 Specifications

• Instrument Range

– Nitrogen 80ppm to 100% Nitrogen @ 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



• Detection Technique

– Nitrogen Thermal Conductivity (TC Cell) Detector

• Furnace Resistance Primary and Secondary up to 1050oC max

• Autoloader 30-position, expandable up to 120

• Electrical Power Requirements

– Instrument 230 V~, 50/60 Hz, single phase, 12A

FP628 Series Specifications (cont.)



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



• 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 samplemass = longer time…)

Samples/Hour

• FP628 Series 14

• Competitor N model 7

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

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.

FP628 Advantages



FP628 Series Software• LECO Windows®-based operating software

– Seamless management of data and

detector plots – Integrated control charts and statistical

calculations



FP628 Series Software

• LECO Windows-based operating software

– Monitor real-time internal component

readings

– Expanded interactive diagnosticscreens aiding

• Troubleshooting

• Improve serviceability



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)



FP628 Calibration

Wide Dynamic Range Calibration

– ~50 mg to ~350 mg EDTA

• 1.0 to 33.5 mg N

• Linear curve type



CN628 Blanks• Low Consistent Blank

– ~3 ppm Nitrogen Std Dev



FP628 Data502-563 Corn Flour Sample Data

– ~250 mg sample mass

– EDTA Calibration

– Cert values:• 1.46 +/- 0.02 % N



FP628 Data502-563 Corn Flour Sample Data



– Cert values:• 1.46 +/- 0.02 % N



FP628 Data

Glycine Solution Sample Data



– Expected value:• 0.1 % N



FP628 Data

Ammonium Sulfate Sample Data



– Theoretical value:• 21.2 % N



CHN628 Series

Elemental Analysis by Combustion

Unparalleled Capabilities



• 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

Leco Macro Nitrogen Determination



Leco Instruments UK Ltd

Thanks for L istening

Michael Reaney

If you require further information please feel free to contact the Leco stand

APA Conference 2011 Presentation Leco

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