TruSpec MethodologyTruSpec Methodology

••High Temperature CombustionHigh Temperature Combustion

••Byproduct removalByproduct removal

••Ballast collectionBallast collection

••SamplingSampling

••Gas IsolationGas Isolation

••MeasurementMeasurement

••Signal ProcessingSignal Processing

••Operational ControlsOperational Controls

High Temperature CombustionHigh Temperature Combustion

••Heat + Oxygen = CombustionHeat + Oxygen = Combustion

••Combustion is an Oxidative Reduction ProcessCombustion is an Oxidative Reduction Process

––C + OC + O22= CO= CO22

––S + OS + O22 = SO= SO22, ,

––H + OH + O22 = H= H22O, O,

––N+ON+O22 = NO= NOxx, ,

––Mineral and Metallic elements = Particulate OxidesMineral and Metallic elements = Particulate Oxides

Combustion ProcessCombustion Process

••Resistance Furnace @ 850Resistance Furnace @ 850ooC to 950C to 950ooCC

••99.99% UHP Oxygen @ defined flows99.99% UHP Oxygen @ defined flows

••0.15g to 1.00g encapsulated sample0.15g to 1.00g encapsulated sample

*ParticleFilter

*Particle*ParticleFilterFilter

ParticleFilter

ParticleParticleFilterFilter

OO22

30 psi30 psi

Low FlowLow FlowLow Flow

Med. FlowMed. FlowMed. Flow

High FlowHigh FlowHigh Flow

Comb. Flow

Comb. Comb. FlowFlow

RestrictorRestrictor

*QuartzSteelWool

*Quartz*QuartzSteelSteelWoolWool

*Precooler*Pre*Pre

coolercooler

*TECooler

*TE*TECoolerCooler **High

CarbonCell

**High**HighCarbonCarbon

CellCell

BallasBallas

tt

*Not used with CHN*Not used with CHN

**Hydrogen cell Used on CHN**Hydrogen cell Used on CHN

Combustion SequenceCombustion Sequence

••Sample weighed and logged inSample weighed and logged in

••Sample loaded, Analyze clickedSample loaded, Analyze clicked

••Combustion area purgedCombustion area purged

••Sample dropped into crucibleSample dropped into crucible

••Gases collected in ballastGases collected in ballast

••Combustion ends when ballast Combustion ends when ballast

pressure equals 1050mmpressure equals 1050mm

Ballast StabilizationBallast Stabilization

••Ballast pressure equals 1100mm Ballast pressure equals 1100mm

stabilization beginsstabilization begins

••Flows stopFlows stop

••Gases isolated in ballastGases isolated in ballast

••Gases equilibrate for 20 secondsGases equilibrate for 20 seconds

Combustion Gas SamplingCombustion Gas Sampling

••Gases released through Gases released through

Carbon Low cell and aliquotCarbon Low cell and aliquot

••Aliquot Fill time complete Aliquot Fill time complete

••Sampling completeSampling complete

BallastBallastBallast

Low CarbonLow Carbon

CellCell

Aliquot Aliquot

Sample ValveSample Valve

Aliquot Aliquot DoseDose

BallastBallast

Output ValveOutput Valve

PressurePressure

SenseSense

3cc loop3cc loop

ExhaustExhaust

HydrogenHydrogen

CellCell

Hydrogen Hydrogen -- Carbon MeasurementCarbon Measurement

••IR Baseline delay completeIR Baseline delay complete

••IR Baseline Time completeIR Baseline Time complete

••IR Reference taken IR Reference taken

••IR Stop Flow completeIR Stop Flow complete

••IR Stabilization completeIR Stabilization complete

••Final output takenFinal output taken

Reference Reference -- Final = mg contentFinal = mg content

mg Content * Standard Cal. mg Content * Standard Cal. -- Blank Blank

* Drift / weight * 100 = %* Drift / weight * 100 = %

BallastBallastBallast

Low CarbonLow Carbon

CellCell

Aliquot Aliquot

Sample ValveSample Valve

Aliquot Aliquot DoseDose

BallastBallast

Output ValveOutput Valve

PressurePressure

SenseSense

3cc loop3cc loop

ExhaustExhaust

HydrogenHydrogen

CellCell

Solid State Infrared DetectionSolid State Infrared Detection

••6 inch Hydrogen Cell6 inch Hydrogen Cell

••3 inch Carbon Low Cell3 inch Carbon Low Cell

••0.7 inch Carbon High Cell0.7 inch Carbon High Cell

••Tungsten Filament source operating @ 900Tungsten Filament source operating @ 900ooCC

••Caf windows at each end of measure chamberCaf windows at each end of measure chamber

••4.274.27µµm COm CO22 filter, 6.3 Hfilter, 6.3 H22O O µµm filterm filter

••Radially Arranged Thermopile Detector Radially Arranged Thermopile Detector

Solid State Infrared DetectionSolid State Infrared Detection

Hydrogen / Carbon Signal OutputHydrogen / Carbon Signal Output

••Reference ~4.00 voltsReference ~4.00 volts

••Gas sampledGas sampled

••Decrease in output = contentDecrease in output = content

5.05.0

4.04.0

3.03.0

2.02.0

1.01.0

0.500.50

0.400.40

0.300.30

0.200.20

0.00.0

Reference outputReference output

Final outputFinal output

BaselineBaseline OffsetOffset

Gas SeparationGas Separation

••Gases swept into flow streamGases swept into flow stream

••Copper / NCopper / N--Catalyst removes OCatalyst removes O22 reduces NOreduces NOxx to Nto N22

••Lecosorb / Anhydrone removes COLecosorb / Anhydrone removes CO22 and Hand H22OO

AliquotAliquotAliquot3cc loop3cc loop

ParticleFilter

ParticleParticleFilterFilter

5InletSV-2InletInletSVSV--22

ExhaustSV-1

ExhaustExhaustSVSV--11

LecosorbAnhydroneLecosorbLecosorb

AnhydroneAnhydroneCu CatalystCu CatalystCu Catalyst6

FlowControl

FlowFlowControlControl3

HeHe

30 psi30 psi LowFlowLowLowFlowFlow

HighFlowHighHighFlowFlow

TCCellTCTCCellCell

12 psiregulator

12 psi12 psiregulatorregulator

44 11FlowMeterFlowFlowMeterMeter

LecosorbAnhydroneLecosorbLecosorb

AnhydroneAnhydrone

77

Thermal Conductive DetectionThermal Conductive Detection

••Gases contain unique Gases contain unique

conductive propertiesconductive properties

••The rate heat is drawn from The rate heat is drawn from

a body is proportional to the a body is proportional to the

amount of a selected gas presentamount of a selected gas present

••He = 33 cal. / sec.He = 33 cal. / sec.

••NN22= 5.6 cal / sec.= 5.6 cal / sec.

••OO22 = 5.7 cal. / sec.= 5.7 cal. / sec.

••COCO22= 3.3 cal. / sec.= 3.3 cal. / sec.

••SOSO22= 1.6 cal. / sec.= 1.6 cal. / sec.

••Ar = 3.8 cal. / sec.Ar = 3.8 cal. / sec.

••HH22O= 4.0 cal. / sec.O= 4.0 cal. / sec.

TC Cell RequirementsTC Cell Requirements

••Isolation of gases Isolation of gases

••Stable flowStable flow

••Stable environmentStable environment

••Stable currentStable current

Measure flow 400 cc /min.Measure flow 400 cc /min.

Reference flow 35 cc /min.Reference flow 35 cc /min.

Insulated compartmentInsulated compartment

Filament Filament

Supply 90 ma.Supply 90 ma.

Nitrogen MeasurementNitrogen Measurement

••TC Stable Comparator CompleteTC Stable Comparator Complete

••TC Baseline Delay CompleteTC Baseline Delay Complete

••TC Baseline time CompleteTC Baseline time Complete

••Baseline taken Measurement starts Cell offset Baseline taken Measurement starts Cell offset

relative to mg / sec. Nrelative to mg / sec. N22

Time

mg

. N

2

Final ResultFinal Result

••Total mg content Total mg content -- blank blank

*calibration * K factor / weight *calibration * K factor / weight

-- atmospheric blank *100 = % Natmospheric blank *100 = % N

••N * Pr factor = % PrN * Pr factor = % Pr

48.32%

System BlankSystem Blank

••A measurable gas from a source other than the sampleA measurable gas from a source other than the sample

••Primary sources effecting Nitrogen are NPrimary sources effecting Nitrogen are N22 or Ar from or Ar from

Oxygen supplyOxygen supply

••Primary sources effecting Carbon and Hydrogen are Primary sources effecting Carbon and Hydrogen are

hydrocarbons from Oxygen supply hydrocarbons from Oxygen supply

••Other sources effecting Nitrogen are OOther sources effecting Nitrogen are O22 or COor CO22

if reagents are depletedif reagents are depleted

Analysis Method ParametersAnalysis Method Parameters

••Sample SizeSample Size––50mg to1.5g or 20mg to 50mg50mg to1.5g or 20mg to 50mg

••Combustion TemperatureCombustion Temperature

––950950ooCC

••Afterburner TemperatureAfterburner Temperature

––850850ooCC

••Element SelectionElement Selection

––Carbon and/or NitrogenCarbon and/or Nitrogen

Analysis Method ParametersAnalysis Method Parameters

••N Comparator LevelN Comparator Level

––1.0%1.0%

••Nitrogen Endline TimeNitrogen Endline Time

––0 to 2 average slope0 to 2 average slope

••C, H & N Conversion FactorC, H & N Conversion Factor

––User DefinedUser Defined

••C, H & N Significant DigitsC, H & N Significant Digits

––1 to 51 to 5

••C, H & N Calibration, Drift and BlankC, H & N Calibration, Drift and Blank

Analysis Method ParametersAnalysis Method Parameters

••IR Analysis Stabilize ComparatorIR Analysis Stabilize Comparator

––Average slope of 0 to 5Average slope of 0 to 5

••IR Baseline Delay TimeIR Baseline Delay Time

––0 to 30 Seconds0 to 30 Seconds

••IR Baseline TimeIR Baseline Time

––0 to 30 Seconds0 to 30 Seconds

••IR Pressure StabilizationIR Pressure Stabilization

––Average slope 0 to 2Average slope 0 to 2

Analysis Method ParametersAnalysis Method Parameters

IR Stop flow timeIR Stop flow time

––0 to 20 seconds0 to 20 seconds

••TC Analysis Stabilize TC Analysis Stabilize

ComparatorComparator

––Average Slope 0 to 2Average Slope 0 to 2

••TC Baseline Delay timeTC Baseline Delay time

––0 to 30 seconds0 to 30 seconds

••TC Baseline TimeTC Baseline Time

––0 to 30 Seconds0 to 30 Seconds

Burn ProfileBurn Profile••Up to 6 stepsUp to 6 steps

••Flow Profile used to provide the correct Flow Profile used to provide the correct

amount of oxygen to the sampleamount of oxygen to the sample

••Profile based on Profile based on

combustion progresscombustion progress

••Requirements are...Requirements are...

a ) Sufficient Oxygen for a ) Sufficient Oxygen for

complete combustioncomplete combustion

b ) Efficient delivery of b ) Efficient delivery of

gases to ballastgases to ballast

4.5 lpm4.5 lpmHigh Flow

High Flow

1.0 lpm1.0 lpmMed. Flow

Med. Flow

Burn 1 Burn 2

0.3 lpm

0.3 lpm Low Flow

Low Flow

Ballast ParametersBallast Parameters

••Equilibrate timeEquilibrate time

––0 to 200 seconds 20 seconds typical0 to 200 seconds 20 seconds typical

••Aliquot fill timeAliquot fill time

––0 to 60 seconds 20 seconds typical0 to 60 seconds 20 seconds typical

••Aliquot pressure stabilization timeAliquot pressure stabilization time

––0 to 60 seconds 5 seconds typical0 to 60 seconds 5 seconds typical

Filters and ReagentsFilters and Reagents

••Quartz / Steel Wool: Quartz / Steel Wool:

––Replace if quartz wool is coated with dust Replace if quartz wool is coated with dust

or steel wool is heavily rustedor steel wool is heavily rusted

••Lecosorb / AnhydroneLecosorb / Anhydrone

––Lecosorb lightens when depletedLecosorb lightens when depleted

••Copper / NCopper / N--CatalystCatalyst

––Replace on count or when blanks increaseReplace on count or when blanks increase

Quartz Wool / Steel WoolQuartz Wool / Steel Wool

••Quartz Wool removes particulatesQuartz Wool removes particulates

••Dust will coat quartz woolDust will coat quartz wool

••Steel Wool removes corrosive saltsSteel Wool removes corrosive salts

••Steel Wool will rust or turn blackSteel Wool will rust or turn black

These tubes are empty for CHNThese tubes are empty for CHN

Particle FilterParticle Filter

••Particle Filter removes salts Particle Filter removes salts

that condense in flow streamthat condense in flow stream

••Replace when extremely dirty Replace when extremely dirty

or Bimonthlyor Bimonthly

Lecosorb / AnhydroneLecosorb / Anhydrone

••Lecosorb is NaOH on KaolinLecosorb is NaOH on Kaolin

••NaOH absorbs CONaOH absorbs CO22 and releases Hand releases H2200

••Anhydrone absorbs HAnhydrone absorbs H22OO

Incoming ScrubberIncoming Scrubber

Measure Stream AbsorberMeasure Stream Absorber

Copper / N Copper / N -- CatalystCatalyst

••Copper removes excess oxygen Copper removes excess oxygen

and reduces NOand reduces NOxx to Nto N22

••N N -- Catalyst reduces tightly Catalyst reduces tightly

bonded NObonded NOxx to Nto N22

••Copper turns black when depletedCopper turns black when depleted

Monthly MaintenanceMonthly Maintenance

••Repack secondary furnace tubeRepack secondary furnace tube

••1500 analyses (based on 200 mg samples) 1500 analyses (based on 200 mg samples)

or when restrictedor when restricted

VacuumVacuumAttachmentAttachment

614614--961961--010010Porous CruciblePorous Crucible

2 Quartz 2 Quartz Wool Strips Wool Strips

2 Quartz 2 Quartz Wool Strips Wool Strips

40cc40ccAlumina OxideAlumina OxidePelletsPellets

30cc30ccFurnace ReagentFurnace Reagent

30cc Magnesium30cc MagnesiumOxide BeadsOxide Beads

2 Quartz 2 Quartz Wool Strip Wool Strip

HoneycombHoneycombCeramicCeramic

TruSpec DeterminatorTruSpec Determinator

ByBy

For More InformationFor More Information

Contact LECO at:Contact LECO at:

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Email: Email: info@leco.cominfo@leco.com

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