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
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